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Invisiblesam.larone
Registered: 01/15/09
Posts: 373
synthesizing LSD *DELETED*
    #9613253 - 01/15/09 07:45 AM (15 years, 3 months ago)

Post deleted by sam.larone

Reason for deletion: .

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Invisibleold mushmellow
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Re: synthesizing LSD [Re: sam.larone]
    #9613259 - 01/15/09 07:48 AM (15 years, 3 months ago)

no

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OfflinePreparationH
apply daily


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Re: synthesizing LSD [Re: old mushmellow]
    #9613263 - 01/15/09 07:50 AM (15 years, 3 months ago)

lol your an optimist.

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Invisiblesam.larone
Registered: 01/15/09
Posts: 373
Re: synthesizing LSD *DELETED* [Re: PreparationH]
    #9613266 - 01/15/09 07:51 AM (15 years, 3 months ago)

Post deleted by sam.larone

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Invisibleold mushmellow
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Re: synthesizing LSD [Re: sam.larone]
    #9613267 - 01/15/09 07:52 AM (15 years, 3 months ago)


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OfflineTreeMoss
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Re: synthesizing LSD [Re: PreparationH]
    #9613276 - 01/15/09 07:57 AM (15 years, 3 months ago)

Ya, mostly since that is your first post and it could be illegal to guide someone through the process........especially with pictures.

Go to school, learn chemistry........get access to the things needed, or make them yourself........read shulgin and there are tons of books from the sixties telling just how to do what you are asking...as easily as it can be done........google works too.....or other threads.

But mostly, that is a sketchy first post.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Invisiblesam.larone
Registered: 01/15/09
Posts: 373
Re: synthesizing LSD *DELETED* [Re: TreeMoss]
    #9613291 - 01/15/09 08:03 AM (15 years, 3 months ago)

Post deleted by sam.larone

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Offlinekrypto2000
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Re: synthesizing LSD [Re: sam.larone]
    #9613293 - 01/15/09 08:05 AM (15 years, 3 months ago)

Expect to spend 1000$+ on materials alone. Not counting the knowledge you must gain and dangers involved if you don't know what you are doing. This definitely doesn't seem the task for you. Be happy you can find LSD at all, many can't.

Maybe grow some mushrooms, extract some mescaline, or try some morning glory/hwbr.

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Invisibleold mushmellow
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Re: synthesizing LSD [Re: sam.larone]
    #9613297 - 01/15/09 08:06 AM (15 years, 3 months ago)

Even with a background in organic chemistry the process is difficult, the equipment is expensive, and the risk of poisoning is real. A skilled mentor is highly suggested. Grow mushies!

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Invisibletruffleupagus
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Re: synthesizing LSD [Re: sam.larone]
    #9613328 - 01/15/09 08:16 AM (15 years, 3 months ago)

So you hate chemistry but you want to synthesize lsd?  LOLZ

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Invisiblejohnm214
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Re: synthesizing LSD [Re: sam.larone]
    #9613329 - 01/15/09 08:16 AM (15 years, 3 months ago)

Read one of the other million posts on the subject, ignore the naysayers, and then come back when you have something specific to discuss.

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OfflineTreeMoss
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Re: synthesizing LSD [Re: krypto2000]
    #9613353 - 01/15/09 08:27 AM (15 years, 3 months ago)

Ya grow mushrooms it is safer and easier....but LSD is not that hard or impossible......the equipment isn't even that expensive compared to the result if you succeed.......or if you find that it is worth doing just for yourself to have a very long lasting supply.

Culturing ergot and getting ET isn't that hard but takes about a month, finding a good source of ergot can be difficult depending on where you live.  I have been trying to find records of local infestations myself, spores have traveled around and there are more than one strain of ergot that makes what you are looking for.

The equipment isn't cheap but it is legal and easy to get without getting watched.

The chemicals are not legal or easy to obtain, I would make them myself as that is actually way easier than trying to rip off a place and having to deal with the investigation that could fallow (depending on inventory checks if something "slips" off the shelf).

Diethylamine is a secondary amine with the molecular structure CH3CH2NHCH2CH3. It is a flammable, strongly alkaline liquid. It is miscible with water and ethanol. As a liquid it has a dark brown color due to impurities, however when distilled it is colorless. It is volatile and has a strong unpleasant odor.

Diethylamine is manufactured from ethanol and ammonia and is obtained together with ethylamine and triethylamine. It is used as a corrosion inhibitor and in the production of rubber, resins, dyes and pharmaceuticals.

Diethylamine is a corrosive chemical and contact with skin may cause irritation or burns.

SYNTHESIS : A solution of 6.7 g KOH in 100 mL H2O, under an inert atmosphere and magnetically stirred, was brought to 75 °C, and 10 g ergotamine tartrate (ET) added. The reaction mixture turned yellow as the ergotamine went into solution over the course of 1 h. The stirring was continued for an additional 3 h. The reaction mixture was cooled to about 10 °C with an external ice bath, and acidified to a pH of about 3.0 by the dropwise addition of 2.5 N H2SO4. White solids started to appear early in the neutralization; approximately 60 mL of sulfuric acid was required. The reaction mixture was cooled overnight, the solids removed by filtration, and the filter cake washed with 10 mL Et2O. The dry solids were transferred to a beaker, suspended in 50 mL 15 % ammonia in anhydrous ethanol, stirred for 1 h, and separated by decantation. This extraction was repeated, and the original decantation and the second extract combined and filtered to remove a few hundred milligrams of unwanted solids. The clear filtrate was stripped of solvent under vacuum, the residual solids dissolved in 50 mL of 1% aqueous ammonia, and this solution was acidified as before with 2.5 N H2SO4. The precipitated solids were removed by filtration and washed with Et2O until free of color. After drying under vacuum to a constant weight, there was obtained 3.5 g of d-lysergic acid hydrate, which should be stored in a dark, sealed container.

A suspension of 3.15 g d-lysergic acid hydrate and 7.1 g of diethylamine in 150 mL CHCl3 was brought to reflux with stirring. With the external heating removed, there was added 3.4 g POCl3 over the course of 2 min, at a rate sufficient to maintain refluxing conditions. The mixture was held at reflux for an additional 5 min, at which point everything had gone into solution. After returning to room temperature, the solution was added to 200 mL of 1 N NH4OH. The phases were separated, the organic phase dried over anhydrous MgSO4, filtered, and the solvent removed under vacuum. The residue was chromatographed over alumina with elution employing a 3:1 C6H6/CHCl3 mixture, and the collected fraction stripped of solvent under hard vacuum to a constant weight. This free-base solid can be recrystallized from benzene to give white crystals with a melting point of 87-92 °C. IR (in cm-1): 750, 776, 850, 937 and 996, with the carbonyl at 1631. The mass spectrum of the free base has a strong parent peak at mass 323, with sizable fragments at masses of 181, 196, 207 and 221.

This base was dissolved in warm, dry MeOH, using 4 mL per g of product. There was then added dry d-tartaric acid (0.232 g per g of LSD base), and the clear warm solution treated with Et2O dropwise until the cloudiness did not dispel on continued stirring. This opaqueness set to a fine crystalline suspension (this is achieved more quickly with seeding) and the solution allowed to crystallize overnight in the refrigerator. Ambient light should be severely restricted during these procedures. The product was removed by filtration, washed sparingly with cold methanol, with a cold 1:1 MeOH/Et2O mixture, and then dried to constant weight. The white crystalline product was lysergic acid diethylamide tartrate with two molecules of methanol of crystallization, with a mp of about 200 °C with decomposition, and weighed 3.11 g (66%). Repeated recrystallizations from methanol produced a product that became progressively less soluble, and eventually virtually insoluble, as the purity increased. A totally pure salt, when dry and when shaken in the dark, will emit small flashes of white light.

Find sources for your materials, write up a pre-lab and price everything and get it done.....it is doable but not an "easy" thing.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Invisibleold mushmellow
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Re: synthesizing LSD [Re: TreeMoss]
    #9613378 - 01/15/09 08:38 AM (15 years, 3 months ago)

It's easier to find the dude with the sheets.

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OfflineTreeMoss
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Re: synthesizing LSD [Re: old mushmellow]
    #9613392 - 01/15/09 08:41 AM (15 years, 3 months ago)

Quote:

old mushmellow said:
It's easier to find the dude with the sheets.




Directions please!


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Invisibleold mushmellow
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Re: synthesizing LSD [Re: TreeMoss]
    #9613408 - 01/15/09 08:44 AM (15 years, 3 months ago)

nearest dead show!

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OfflineTreeMoss
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Re: synthesizing LSD [Re: old mushmellow]
    #9613456 - 01/15/09 09:01 AM (15 years, 3 months ago)

Ha ya well they aren't coming around me, I'd have to go to the next state but really........I don't think I can just walk up to anyone and ask around about that.........I am not a very social person and people are kinda iffy.......well, either too cool or way not cool....just goofy.

But hey, I am usually the one asking around but sometimes some shows things just don't find me.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Invisibleold mushmellow
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Re: synthesizing LSD [Re: TreeMoss]
    #9613472 - 01/15/09 09:06 AM (15 years, 3 months ago)

I had a friend dump some pyramid windowpane on me recently so I know its around. just look for the guy with the endless smile on his face.:D

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OfflineCepheus
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Re: synthesizing LSD [Re: sam.larone]
    #9615183 - 01/15/09 03:00 PM (15 years, 3 months ago)

Buy the book TiHKAL. Instructions in there for the synthesis of most drugs worth doing :grin:.


--------------------
"I only ever hope to reach equilibrium, in Nature's matrix, in line with the meridian" ~ Jehst

:sun: "...and I know that I have to keep breathing, as tomorrow the sun will rise, who knows what the tide will bring?" :sun:

Free Spore Ring Europe
Send any spare spore prints you might have and help the distribution :grin:

Open Source. Freedom.  GNU/Linux

Addicting is not a word.

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Offlineiateshaggy
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Re: synthesizing LSD [Re: Cepheus]
    #9617373 - 01/15/09 08:18 PM (15 years, 3 months ago)

lol, not gonna read the whole thread, but go to an ivy league school and major in organic chemistry, then maybe go on to get a masters and maybe even a doctorate, make a ton of money to invest in the process and make some connections in the pharmaceutical industry to hook u up w/ some erogotamine tartrate.  then find an abandoned missle silo in kansas and hook it up till the D34 catch u.  ask pickardy for pictures, now that he is in prison, i'm sure he's a lot cooler about sharing them.


--------------------
You are a filipina sex goddess who wants to fuck me until I fall asleep, so then you can tickle my balls and see if the legend of my diamond filled nutsuck is true.  I am a white man from costa rica, who smells like lime jello.


I can flash/jtag/repair 360's, pm for details.

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OfflinePoiesis
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Re: synthesizing LSD [Re: johnm214]
    #9619771 - 01/16/09 08:27 AM (15 years, 3 months ago)

Quote:

johnm214 said:
Read one of the other million posts on the subject, ignore the naysayers, and then come back when you have something specific to discuss.




Second.

While the OP is doing his homework, I will prepare a picture of how to stir.  Does it need to be clockwise or counterclockwise?  I can never remember.


--------------------

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Offlineiateshaggy
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Re: synthesizing LSD [Re: Poiesis]
    #9619829 - 01/16/09 08:41 AM (15 years, 3 months ago)

Quote:

Poiesis said: Does it need to be clockwise or counterclockwise?  I can never remember.



depends, are u in the northern or souther hemisphere?


--------------------
You are a filipina sex goddess who wants to fuck me until I fall asleep, so then you can tickle my balls and see if the legend of my diamond filled nutsuck is true.  I am a white man from costa rica, who smells like lime jello.


I can flash/jtag/repair 360's, pm for details.

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OfflinePoiesis
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Re: synthesizing LSD [Re: iateshaggy]
    #9623285 - 01/16/09 08:35 PM (15 years, 3 months ago)

Of course.  No wonder I keep forgetting.  I am right on the equator.

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Invisiblearainbow
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Re: synthesizing LSD [Re: Poiesis]
    #9635005 - 01/18/09 10:10 PM (15 years, 2 months ago)

go to a rainbow gathering there is pounds I mean pounds of the stuff being given away

I don't do acid unless I can do at least 15 hits
or 2000mcg liquid

even at that I'm offered more than I want to do
at every gathering I go to

some how I became a high holy and get treated like a king at the gatherings by other high holys


--------------------
There is more joy in heaven over one of us perfected,
  than over ninety-nine naturally evolved angels.

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OfflineTreeMoss
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Re: synthesizing LSD [Re: arainbow]
    #9643970 - 01/20/09 06:37 AM (15 years, 2 months ago)

Quote:

arainbow said:
go to a rainbow gathering there is pounds I mean pounds of the stuff being given away

I don't do acid unless I can do at least 15 hits
or 2000mcg liquid

even at that I'm offered more than I want to do
at every gathering I go to

some how I became a high holy and get treated like a king at the gatherings by other high holys




I've never seen acid at a gathering although I would suspect it's floating around.  I ran into other things but no acid yet, then again it's only been about 4 gatherings that I have been too.

I thought it was pretty annoying how some people just walk around yelling to be dosed.  Maybe some day I will be in the right place at the right time.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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OfflineSheerTerror
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Re: synthesizing LSD [Re: sam.larone]
    #9654611 - 01/21/09 07:42 PM (15 years, 2 months ago)

Its basically impossible because of the chemicals being so hard to obtain and because of all the chemistry knowledge and experience needed.

I wonder how much LSD there is in other countries where the chemicals needed aren't strictly regulated.

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Invisiblejohnm214
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Re: synthesizing LSD [Re: SheerTerror]
    #9655157 - 01/21/09 09:10 PM (15 years, 2 months ago)

fail

you need no chemistry knowledge, and I could get the chemicals and I don't have a degree or work anywhere with chemicals presently

follow tihkal and look up the words you don't understand

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OfflineSheerTerror
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Re: synthesizing LSD [Re: johnm214]
    #9655964 - 01/21/09 11:14 PM (15 years, 2 months ago)

well then lets do it up.

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Offlinezouden
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Re: synthesizing LSD [Re: johnm214]
    #9657135 - 01/22/09 05:37 AM (15 years, 2 months ago)

Really? Ergotamine? You need a prescription to get that here.


--------------------
I know... that just the smallest
                                                part of the world belongs to me
You know... I'm not a blind man
                                                    but truth is the hardest thing to see

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OfflineTreeMoss
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Re: synthesizing LSD [Re: zouden]
    #9657262 - 01/22/09 06:53 AM (15 years, 2 months ago)

You would have to find it in bulk and in raw form, it's usually with caffeine and I have no idea how to separate that easily and purely....any amount would mess things up really badly.

Easier for most that can find a culture to just make gallons of the stuff.  The Diethylamine can be distilled easily, not sure how to separate it from what else is produced....but surely some research could indicate how to do that.

there are some really good books out there on how to make LSD but back then the chemicals were easier to get so you would have to make those if you didn't have a supplier........making it in Mexico would be a piece of cake if you knew the right people.....but if you didn't you would have some problems and really might anyhow due to drug trade politics..........better really know the top people of whatever area you are in.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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OfflinePoiesis
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Re: synthesizing LSD [Re: zouden]
    #9657360 - 01/22/09 07:52 AM (15 years, 2 months ago)

Quote:

zouden said:
Really? Ergotamine? You need a prescription to get that here.




Ergotamine is not the only starting point.
Many ergot alkaloids will do.
Extraction of these starting material from c. purpurea would be one way to do it.
Johnm214 is right.


--------------------

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OfflineTreeMoss
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Re: synthesizing LSD [Re: Poiesis]
    #9657377 - 01/22/09 08:01 AM (15 years, 2 months ago)

Quote:

Poiesis said:
Quote:

zouden said:
Really? Ergotamine? You need a prescription to get that here.




Ergotamine is not the only starting point.
Many ergot alkaloids will do.
Extraction of these starting material from c. purpurea would be one way to do it.
Johnm214 is right.





That is how you get ET!  The fact is you would gain chemistry knowledge quickly.........but it is good to know what you are playing around with if you make your own diethylamine and anything else explosive......diethylamine isn't all that different than making ether but you use ammonia instead of acid....and I really would like to make my own ether.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Offlinekrypto2000
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Re: synthesizing LSD [Re: TreeMoss]
    #9657390 - 01/22/09 08:07 AM (15 years, 2 months ago)

What is ether commonly used for? Forgive my ignorance. :confused:

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Invisiblejohnm214
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Re: synthesizing LSD [Re: zouden]
    #9657394 - 01/22/09 08:08 AM (15 years, 2 months ago)

Quote:

zouden said:
Really? Ergotamine? You need a prescription to get that here.




Here as well but, same with prozac.  I'd order it oversees or get a script.  For small scale "I did it" it seems the best way.


1.  Little concern re: impurities that you don't know about

2.  Little concern about similar ergot alkaloids

3.  Easy seperations.


I've never tried, but I'd imagine cafergot is mostly caffeine and ergotamine and that celluslose product and talc.  I would think simple extractions would work.  TLC to verify would be about all the analysis you'd need for presumptive results.


Since sasha was nice enough to write up how to do it, follow and get results.  You can pick any of the other methods too if you like, sasha's just seemed so well-laid-out for a novice.  You wouldn't have to know much at all.  You're just pouring and boiling and stuff.

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InvisibleMisterMuscaria
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Re: synthesizing LSD [Re: arainbow]
    #9657395 - 01/22/09 08:08 AM (15 years, 2 months ago)

BE CAREFUL when starting with ergot, it can be very harmful to the health. Take proper precautions (gloves, mask, full body suit). St.Anthony's fire is no joke!

Quote:

arainbow said:
go to a rainbow gathering there is pounds I mean pounds of the stuff being given away

I don't do acid unless I can do at least 15 hits
or 2000mcg liquid

even at that I'm offered more than I want to do
at every gathering I go to

some how I became a high holy and get treated like a king at the gatherings by other high holys



A few thousand hits? sure...but I wouldnt say lbs at a gathering.

Edited by MisterMuscaria (01/22/09 08:10 AM)

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OfflineTreeMoss
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Re: synthesizing LSD [Re: krypto2000]
    #9657470 - 01/22/09 08:33 AM (15 years, 2 months ago)

Quote:

krypto2000 said:
What is ether commonly used for? Forgive my ignorance. :confused:




Cocaine crystallization......suppose meth and any other crystal as well.

Mescaline too......probably DMT as well.

Anything that requires a non-polar solvent.......but the best flaky cocaine comes from a ether crystal process......it's not even common in Columbia.  I watched on YouTube some guy making cocaine in the jungle and damn, it was tragic.  I'm suprised that he got anything that looked like cocaine at all, I didn't even seem him oxidize it.  He just poured ammonia into the agua rica when it was brown and then it turned white with precipitates (base).


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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OfflineTreeMoss
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Re: synthesizing LSD [Re: MisterMuscaria]
    #9657474 - 01/22/09 08:34 AM (15 years, 2 months ago)

There are so many people at nationals, I've never even smoked good nugs at a national but some decent mids..........I never found that super hot sister in my tent yet either but boy are some around...damn, this one still flashes into my mind sometimes......super hot!


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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InvisibleMisterMuscaria
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Re: synthesizing LSD [Re: TreeMoss]
    #9657481 - 01/22/09 08:37 AM (15 years, 2 months ago)

I smoked good nugs AND found the super hot sister in my tent at my first gathering. At my last gathering I got robbed for everything I had but I smoked the best hash Ive ever smoked.

Edited by MisterMuscaria (01/22/09 08:42 AM)

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Offlinekrypto2000
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Re: synthesizing LSD [Re: TreeMoss]
    #9657506 - 01/22/09 08:48 AM (15 years, 2 months ago)

MMmmm... Me would love some even nicer Mescaline porn(crystals) :smile:

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Re: synthesizing LSD [Re: zouden]
    #9657575 - 01/22/09 09:11 AM (15 years, 2 months ago)

does anyone know how prevalent LSD in other countries like Asia, because the ammount of arrests would show how much there is and if its that obtaining the chemicals in the US is why its not around anymore.

I know john says he can make it but I think that if it is easy to make it would be all over the country again cause there is a huge demand for it and the potency is so high so if the synthesis yeilded a gallon that would equal approx 5,000 hits= $25,000 a synthesis so I'm sure someone would do this if they could.

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Re: synthesizing LSD [Re: SheerTerror]
    #9657598 - 01/22/09 09:16 AM (15 years, 2 months ago)

I know Japan, Russia and India are all having their own LSD movements recently, but I am unsure of China.
Russia even legalized it for research.

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Re: synthesizing LSD [Re: SheerTerror]
    #9657600 - 01/22/09 09:17 AM (15 years, 2 months ago)

I don't think it's cause it's hard. It's costly to start up and has a lot of legal and health risks if you are not very tedious and careful in your practices. Plus, for the knowledge it does require, which I gather really isn't that extensive, most people feel, on top of the aforementioned downsides, that it is just not worth it to invest the time to gain said knowledge.

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Re: synthesizing LSD [Re: SheerTerror]
    #9657694 - 01/22/09 09:43 AM (15 years, 2 months ago)

I said I could make it, I didn't say I could make it for the whole state or whole country.


I'm saying to make the chemical in microscale quantities its no big deal.  Given that that's not to small with LSD's dosage being low its a decent amount- but I was just saying that its not like its some hard procedure or anything you need an education to follow.

Most people are intimidated by chemical synthesises and would think its harder than it is and also couldn't get large scale quantities of precursors.  I've never heard anyone mention the cafergot before me, which is probably revealing of the fact people don't really think about it that much.

They guys that would make large quantities would find their own source- I'm just saying you could make it with a few pills unless the extraction is problematic, but it removes a lot of the trouble in obtaining lysergic acid.

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Re: synthesizing LSD [Re: johnm214]
    #9657969 - 01/22/09 10:45 AM (15 years, 2 months ago)

You guys who say its easy to make must be highly skilled chemists, that or completely stupid. there really is allot more to the process than mixing A to B. Its a tedious and expensive endeavor. The ergotamine tartrate needed for the easiest method runs around $650 for ten grams (it is available from overseas)ergonovine is even more costly. The proper labware runs around $6000 for everything you need including the chromatography. The other reagents need to be pharmaceutical grade (unless you're a hack), Oh, around another $700. Still you need a highly skilled chemist willing to do the dance. Following recipes from books is not a good idea, you need someone who knows the math too. I suppose if you're willing to blow yourself up or cause your arms and legs to fall off after ingesting ergot alkaloids, you should jump right in there and give 'er a go. Otherwise leave it to the highly trained underworld pro's.:chemistry:

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Re: synthesizing LSD [Re: old mushmellow]
    #9657993 - 01/22/09 10:48 AM (15 years, 2 months ago)

Good lord, please brea down the 6000$ figure for equipment please.  You incluing a gc in that or what?


Please explain why you need to be highly skilled.  If you'll read my other posts in other threads I give a layman's explanation of the tihkal procedure- which is "mix this shit, boil, wait, mix, pour" shit like that.


Rather than opine its hard, why not demonstrate such?  (and don't even start with the light sensitive stuff.  Lights have switches.)

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Re: synthesizing LSD [Re: johnm214]
    #9658015 - 01/22/09 10:51 AM (15 years, 2 months ago)

If you understand the chemistry then you know what you need.

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Re: synthesizing LSD [Re: old mushmellow]
    #9658029 - 01/22/09 10:54 AM (15 years, 2 months ago)

It's as expensive as you make it but there are certain basic cost.

Your going to be experienced after you first success (and already on your way just getting to that).

Small batches are the way to go......you need an inert atmosphere but that isn't all to difficult.......I think the most dangerous and hardest part is making your chemicals and finding a good ergot culture and making more of that.

I would think that someone would have a collection of ergot but to get a piece of theirs is sketchy as far as schools and research labs go.

But I read something about an African strain that is potent that invaded most of the world.........recently.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Re: synthesizing LSD [Re: old mushmellow]
    #9658040 - 01/22/09 10:56 AM (15 years, 2 months ago)

Quote:

old mushmellow said:
If you understand the chemistry then you know what you need.




No shit, which is why I know you're just making shit up- why I asked you to justify your claim.


The only way you could justify that is by buying a whole bunch of stuff you don't need.  "Um, I'll take a GC too, need that"

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Re: synthesizing LSD [Re: TreeMoss]
    #9658074 - 01/22/09 11:01 AM (15 years, 2 months ago)

Why go the culture route when ergot pharmaceuticals are available? They save time and money and some of the risk. And you don't have to go through extraction, incubation, and making precursors.

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Re: synthesizing LSD [Re: old mushmellow]
    #9658089 - 01/22/09 11:03 AM (15 years, 2 months ago)

Well ya you could go about it that way or just make it all yourself.

You would get a better deal making it yourself and it's pretty safe to work with.....just don't swim in it!

But do you know how to separate the ET, cause if your going to Mexico surely you could get pure ET but getting it through the border might be a bit more risk than you would want to gamble with.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Re: synthesizing LSD [Re: johnm214]
    #9658108 - 01/22/09 11:06 AM (15 years, 2 months ago)

Yup, I just pull that bullshit right outa my ass. I wonder what the pharmacy college I went to would have to say?

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Re: synthesizing LSD [Re: old mushmellow]
    #9658144 - 01/22/09 11:11 AM (15 years, 2 months ago)

I thought I made it clear I and nobody else should care about your opinion when its not premised upon stated facts or premises.  I also don't care about your unnamed pharmacy college thinks.  Maybe you should ask them to justify your opinion since you seem to have trouble doing so.

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Re: synthesizing LSD [Re: johnm214]
    #9658156 - 01/22/09 11:13 AM (15 years, 2 months ago)

I'm not giving you a lab list, you might hurt yourself, Then I'd feel bad.

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Re: synthesizing LSD [Re: johnm214]
    #9658157 - 01/22/09 11:13 AM (15 years, 2 months ago)

And this debate is really about what?

I see a lot of crap that gets thrown around and it's mostly unwritten ideas that both parties seem to have on the other side of the screen but in opposites of some form.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Re: synthesizing LSD [Re: johnm214]
    #9658164 - 01/22/09 11:14 AM (15 years, 2 months ago)

I think you should attempt the synthesis.

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Re: synthesizing LSD [Re: SheerTerror]
    #9658175 - 01/22/09 11:16 AM (15 years, 2 months ago)

It's a worthwhile thing to attempt in ones life, to a point of success.  But for a sake of argument stupid to do it just for that.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Re: synthesizing LSD [Re: SheerTerror]
    #9658181 - 01/22/09 11:16 AM (15 years, 2 months ago)

Ya, but who's the guinea pig?

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Re: synthesizing LSD [Re: TreeMoss]
    #9658192 - 01/22/09 11:19 AM (15 years, 2 months ago)

Quote:

TreeMoss said:
And this debate is really about what?

I see a lot of crap that gets thrown around and it's mostly unwritten ideas that both parties seem to have on the other side of the screen but in opposites of some form.




He stated some ridiculous number for the value of the equipment to make LSD.  I said it was inaccurate and much too high unless he was including some analytical equipment or something, and he invoked appeals to (unnamed) authority and some stupid claim he goes to school without giving any credentials.



Just saying its not that expensive.  And that he's not shown how it could be.

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Re: synthesizing LSD [Re: johnm214]
    #9658215 - 01/22/09 11:23 AM (15 years, 2 months ago)

Ya it can be a small scale thing......but still not that cheap to really know what you have.......but you could just do more work to be more certain instead of testing what you have at various stages....before salting having the base and that part of testing.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Re: synthesizing LSD [Re: johnm214]
    #9658277 - 01/22/09 11:32 AM (15 years, 2 months ago)

... GOOD LUCK! LOL

Edited by old mushmellow (01/22/09 11:41 AM)

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Re: synthesizing LSD [Re: old mushmellow]
    #9658304 - 01/22/09 11:36 AM (15 years, 2 months ago)

Why are you telling him to do that, that isn't something that promotes knowledge or anything other than your selfish ego.

Very plasmid like of you!  I don't see people with your knowledge encouraging legal use of these drugs and very few go out and do what was shut down in 2000.........in fact nobody yet at that scale.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Re: synthesizing LSD [Re: TreeMoss]
    #9658337 - 01/22/09 11:40 AM (15 years, 2 months ago)

How true I'll edit. sorry man

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Re: synthesizing LSD *DELETED* [Re: TreeMoss]
    #9658346 - 01/22/09 11:43 AM (15 years, 2 months ago)

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Re: synthesizing LSD [Re: sam.larone]
    #9658371 - 01/22/09 11:46 AM (15 years, 2 months ago)

Jeesh I'll incriminate myself if I answer this publicly. I'll PM

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Re: synthesizing LSD *DELETED* [Re: old mushmellow]
    #9658393 - 01/22/09 11:49 AM (15 years, 2 months ago)

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Re: synthesizing LSD [Re: sam.larone]
    #9658425 - 01/22/09 11:54 AM (15 years, 2 months ago)

Base-catalyzed Hydrolysis of Ergocristine to Lysergic Acid
by KrZ


Ergocristine base was obatined, and the subsequent base-catalyzed hydrolysis was a glowing success. The procedure here is very simple. Gloves should be worn at all times. Have a bucket of water to rinse the gloves in before you take them off so you will not contact the skin when trying to remove them, be careful cleaning all glassware.
Procedure

33.5g KOH was dissolved in 500ml dH2O in a 1000ml flask, and the solution was stirred magnetically, heating was commenced and the temperature of the solution was allowed to reach 75°C. 50g of Ergocristine base was added in 2g fractions over a period of 30 minutes. The mix went from clear to a light golden yellow tint over the course of the addition. Everything was in solution after 50 minutes. The reaction was allowed to proceed for a total of 5 hours after complete addition. Heating was removed and the reaction flask placed in a room temp. water bath, and then in an ice bath, until the solution was at 5°C. 325 mL 2.5 N H2SO4 was placed in an addition funnel, the flask placed in the ice-bath and stirred, and the acid was added dropwise. As the volume added reached ~200 mL pH metering was commenced, and addition was halted when the pH reached 3.0, ~50 mL of acid remained in the addition funnel. The flask was sprayed out with a stream of nitrogen, stoppered, wrapped in aluminum foil, and stored at 0°C for 18 hours (dark, of course). The flask was then removed, swirled vigorously to mix the solids, and quickly poured onto the buchner funnel. 100 mL of Et2O was added to the flask, in two fractions, swirled, and poured over the filter cake. The filter cake was placed in a vacuum dessicator in the dark for two hours. The filter cake was scraped into 500 mL NH3/EtOH solution, and the filter paper rinsed with two syringes full of the NH3/EtOH solution. The solution was stirred for 90 minutes (lights off), decanted, the solids re-extracted with a second 500 mL NH3/EtOH fraction (90 min. stirring, lights off), and filtered to remove the remaing solids (weight 1440 mg). The pooled extracts were stripped of solvent under vacuum at the rotovap (lights off, temp. set then left in dark). The solids remaing in the flask were taken up in 500 mL of 1% Aq. Ammonia. 250 mL 2.5 N H2SO4 was placed in the addition funnel, and added slowly with stirring to a beaker containing the extract. The pH was monitored continuously and addition was halted as the pH reached 3.0, the beaker was covered and placed in the refrigerator overnight. The solids were stirred vigorously to suspend them and collected by vacuum filtration. The beaker was swirled with 100 mL Et2O and the briefly suspended solids poured over the filter cake. The filter cake was placed in the vacuum dessicator for two hours (in the dark), and then weighed at 16.48g, placed in a brown glass vial, sprayed with nitrogen, sealed, wrapped in foil, and stored in the freezer at -10°C. The yield equates to 73%.

15% NH3 in EtOH prep.

1000 mL of 15% Ammonia in Anhydrous Ethanol was prepared by the slow addition of NaOH to cold absolute ethanol containg NH4Cl (not dissolved), filtration, and drying of the formed water by adding 0.20g CaO/1g H2O formed, with stirring and cooling. The formed calcium hydroxide was filtered.

Lighting

Regular lighting was used during the reaction. Two red photography lights were used during the rxn workup.

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Re: synthesizing LSD [Re: sam.larone]
    #9658448 - 01/22/09 11:57 AM (15 years, 2 months ago)

Lysergic Acid Diethylamide (LSD) Syntheses
from "Recreational Drugs" by Professor Buzz


Synthesis of Lysergic Acid

By reacting N-benzoyl-3-(B-carboxyethyl)-dihydroindole (see JCS, 3158 (1931) for the preparation of this compound) with thionyl chloride, followed by aluminum chloride gives 1-benzoyl-5-keto-1,2,2a,3,4,5-hexahydrobenzindole. This is then brominated to give the 4-bromo-derivative, which is converted to the ketol-ketone by reacting with methylamine acetone ethylene ketol. This is then hydrolized by acid to yield the diketone and treated with sodium methoxide to convert it to the tetracyclic ketone. Acetylate and reduce this ketone with sodium borohydride to get the alcohol, which is converted to the hydrochloride form, as usual.

The above hydrochloride is treated with thionyl chloride in liquid sulfur dioxide, to produce an amorphous chloride hydro chloride, which is converted to the nitrile with sodium cyanide in liquid hydrogen cyanide. Methanolysis then gives the ester of the nitrile. Alkaline hydrolysis of this last compound, followed by catalytic dehydrogenation in water using a deactivated Raney Nickle catalyst (see JOC. 13, 455 1948) gives dl-lysergic acid.
Total Synthesis Of Lysergic Acid

This is the easiest way to totally synthesize lysergic acid. There are other ways, but after reviewing other methods, I found this to be superior. It is quite complicated and it takes good modern equipment.

JACS, 78, 3087 (1956). 3-Indolepropionic acid, 94.5 g (0.5 mole) is dissolved in 600 ml of water containing 20 g of NaOH. The solution is mixed with 100 g of Raney Nickle catalyst and hydrogenated at room temp in a steel bomb at about 3,500 psi until the uptake of hydrogen stops (about 20-30 hours). Filter off the catalyst and wash it with a little water to remove the product that is clinging to it. Add 85 ml of concd HCl acid to the filtrate, and cool. If your reduction is incomplete, you will now have unreacted starting material separate, and this must be removed by filtration. Benzoylate the filtrate (the Schotten and Baumann method is preferable), using 210 ml of 12 N NaOH 180 ml of benzoyl chloride. Keep the solution alkaline throughout the benzoylation, and keep the temp below 40°C by cooling. When the benzoyl chloride is fully reacted, the reaction mixture is cooled and acidified with 300 ml of HCl acid. Filter the crude product by filtration, wash with water, and extract with four 1 liter portions of hot water. Separate, and crystallize the resulting syrupy product from a few volumes of methanol. Filter and wash with a little cold methanol to get a little over 100 g that melts at 151-153°. This is l-Benzoyl-3-beta-carboxyethyl-2,3-dihydroindole. This can be purchased to eliminate this step.

1-Benzoyl-5-keto-1,2,2a,3,4,5,-hexahydrobenzindole. 118 g of the above product (1-benzoyl-3-B-carboxyethyl-2,3-dihydroindole) is mixed with 200 ml of pure thionyl chloride. This solution is allowed to stand for 30 min, then it is warmed gently for 15-21 min on a steam bath. Excess thionyl chloride is completely evaporated with the temp maintained between 22-26°C in vacuo. The crude acid chloride is dissolved in dry carbon disulfate. This solution is added, in a thin stream, to a well stirred suspension of 240 g of aluminum chloride in 1750 ml of carbon disulfate in a 5,000 cc flask. Note: this must be done under a fume hood. A complex will separate and bog down the stirring device. Heat this mixture under reflux with stirring for 1 hour. Decompose this mixture by adding 500 g of ice, 250 ml of concd HCl acid, and 500 ml of water, all while good stirring is continued. Cooling of this operation is affected by periodic distillation of the carbon disulfate in vacuo. After the decomposition is complete, any remaining carbon disulfate is removed completely in vacuo, and the product is extracted with 2 liters of benzene. The extract is washed well with 500 ml of 2 N NaOH in three portions, and then with water. Dry (with the usual magnesium sulfate), and evaporate to a small volume in vacuo. Add this small volume to several portions of ether to get the ketone to crystallize (add slowly), and filter, then wash with ether to get 85 g of pure title product, mp: 146-147°C.

1-Benzoyl-4-bromo-5-keto-1,2,2a,3,4,5-hexahydrobenzindole. A solution of the above indole (305 g) in 2,200 ml of glacial acetic acid is warmed to 40°C. While the reaction is illuminated with a 250 watt bulb, 352 g of pyridine hydrobromide perbromide is added in portions, over 5 min with shaking. The solution is then heated to 60° and is held between there and 55°C for 30 min. Treat the mixture with carbon, and evaporate to a small volume in vacuo. The residue is taken up with 2,200 ml of chloroform, and wash this solution with several portions of water, dry as above, and concentrate in vacuo. Crystallize the residue from 2,200 ml of 50% acetic acid and 50% ether to get 270 g of title product that melts at 180.5-181.5°C. Another crop can be obtained from concentrating the fltrates. Yield: 30 g of less pure product.

1-Benzoyl-2,2a,3,4-tetrahydro-4-methyl-2-methyl-1,3-dioxolan-2-yl-methyl-aminobenzindol-5-(1H)one. A solution of the last indole product above (270 g) and 307 g of methylaminoacetone ethylene ketol in 4,500 ml of dry benzene is refluxed for 21 hours under a slow stream of nitrogen. The mixture is cooled and 151 g of methylaminoacetone ethylene ketol hydrobromide is filtered off. The filtrate is washed with ice water, then extracted with 2.5 liters of cold dilute HCl acid containing 150 ml of the concd acid. The acid extracts are immediately added to an excess of ice cold dilute NaOH. Extract with 1 1iter of chloroform, dry over magnesium sulfate, treat with carbon and concentrate by evaporation in vacuo. The residual ketol-ketone is crystallized from acetone to yield 220 g, mp: 135-136°C.

5-Keto-4-N-methyl-N-acetonylamino-1,2,2a,3,4,5-hexahydrobenzindole. 20 g of the above product is dissolved in a mixture of 250 ml of concd HCl acid and 250 ml of water, and the solution is kept under nitrogen for 5 days at 37°. Cool the mixture, treat with carbon, filter, and concentrate the filtrate in vacuo to a small volume. Treat the residue with an excess of sodium bicarbonate, extract with cold chloroform, and remove the chloroform by evaporation in vacuo at room temp. The crude diketone is powdered, slurried with 75 ml of benzene-ether, and filtered. Yield: 9.8 g, mp: 105-107°C.

9-keto-7-methyl-4,5,5a,6,6a,7,8,9-octahydroindolo-(4,3)isoquinoline. 25 g of the above product is mixed with 550 ml of absolute ethanol. Stir this mixture under nitrogen and cool to -15° with an external freezing mixture. Sodium methoxide is added (17 g) and the mixture is stirred for 10 min at -10 to -12°. Cool to -25°, and the product is filtered and washed (while still in the funnel) with cold ethanol and ether. Without exposure to air the crude ketone is immediately slurried with a little ice water and filtered. Wash with ice water, ethanol, then ether (all cold) to yield 16 g of product melting at 145-147°.

4-Acetyl-9-keto-7-methyl-4,5,5a,6,6a,7,8,9-octahydroindolo-4,3-quinoline. 24 g of the last product is added to 80 ml of cold acetic anhydride. The mixture is held at 25° for about 5 min, then thoroughly cooled, filtered, and the product (a solid) washed with ether to yield 20.5 g, mp: 169-170°. A second crop is obtained by concentrating the mother liquor by evaporation.

A mixture of the last product (1.0 g) and 10 g of palladium carbon (5%), in 35 ml of xylene, is heated under reflux for 4 hours. The catalyst is filtered and extracted with hot methanol and chloroform. The combined extract filtrates and the initial filtrate are combined and evaporated in vacuo. The residue is recrystallized from water to give 0.6 g of a monohydrate product that melts at 255-256°. This product is called 4-acetyl-4,5,5a,6-tetrahydro-9-hydroxy-7-methylindolo-(4,3fg)-quinolinium hydroxide betaine.

4-Acetyl-9-hydroxy-7-methyl-4,5,5a,6,7,8,9,10-octahydroindolo-(4,3fg)-quinoline. 1 g of the above betaine in a mixture of 20 ml of ethanol and 5 ml of water, is treated with 0.08 g of sodium borohydride, and this solution is refluxed for 10 min and kept at 25° for 1 hour after the reflux is finished. The solvent is distilled off, and the residue is taken up in a mixture of chloroform and water. The chloroform solution is separated, dried as above, and then the solvent is distilled off. The residue is recrystallized from a nitromethane-ethyl acetate mixture to yield 0.2 g (21%), mp 193-196°. Not only is this a small scale, but it is a poor yield, requiring you to perform it several times to get enough product to perform the next step. When you have more than enough, convert the product into its hydrochloride form by dissolving in dry methanol and precipitating with dry hydrogen chloride.

4-acetyl-9-chloro-7-methyl-4,5,5a,6,6a,7,8,9-octahydroindolo-(4,3fg)-quinoline hydrochloride. 3.1 g of the above product in its hydrochloride form is dissolved in 75 ml of liquid sulfur dioxide contained in a glass lined, high pressure bomb, or autoclave. Thionyl chloride (1.2 ml) is added and the vessel is sealed and kept at 25° for 6 hours. Vent the vessel carefully and remove the mixture. Evaporate the sulfur dioxide while keeping the volume of the solution constant by the slow addition of dry ether. The amorphous chloro hydrochloride is filtered, washed with ether (dry) and dried by evaporating in vacuo to give 3.5 g of product, mp:130-135°.

4-Acetyl-9-cyano-7-methyl-4,5,5a,6,6a,7,8,9-octahydroindolo-(4,3fg)-quinoline. 40 g of dry, powdered sodium cyanide, is added to ice cold liquid hydrogen cyanide and stirred gently with ice bath cooling. Speed up the stirring, continue the cooling, and add 7.5 g of the amorphous product directly above. Continue stirring for 30 min, then the hydrogen cyanide is distilled under enough reduced pressure to keep it coming over the condenser at a temp below 10-12°. The residue is mixed with chloroform and ice water, and the resulting mixture is filtered. The organic layer of the filtrate is separated and the aqueous layer is extracted with two separate portions of chloroform. The combined extracts (this would include the separated chloroform, as usual) are dried over magnesium sulfate, decolorized, and the solvent removed by distillation in vacuo. Crystallize the product in ethyl acetate. Yield: 3.3 g, mp: 173-174°. Recrystallize again for extra purity.

9-Carbomethoxy-7-methyl-4,5,5a,6,6a,7,8,9-octahydroindolo-(4,3fg)-quinoline. 1 g of the last product is mixed with 15 ml of methanol and 0.25 ml of water. With external (ice bath) cooling add 2 ml of concd sulfuric acid slowly. Seal this solution in a high pressure bomb with a glass liner (or in a glass tube taking safety precautions in case of explosion) with a nitrogen atmosphere, and heat at 100° for 23-24 hours. Note: I have seen a big pressure cooker (like gramma cans peas with) work for some of these bomb procedures. I do not recommend it, but here is how to do it right, if you feel you must. Use only the great big heavy duty models, in excellent condition, set the pop off (relief valve) for near maximum position; never, ever tamper or modify this valve to get more pressure. Put the product in a glass beaker, put it in the cooker, flush with nitrogen, heat and stay in a different house during the reaction. Carefully turn off heat, notice or record pressure gauge after time has elapsed. Wait until pressure drops noticeably, bleed off remaining pressure and get product.

Treat the mixture with decolorizing carbon and then evaporate in vacuo to 10 ml. Pour onto a mixture of 30 ml of chloroform, ice, and 10 g of sodium bicarbonate. Separate the chloroform layer, and extract the aqueous phase with three 10 ml portions of chloroform. The combined chloroforms are dried, evaporated to dryness in vacuo, and the product is crystallized from benzene to give 1/2 g of product that melts at 159-160°. You may purify more by recrystallizing from ethyl acetate. This is not very much product. As with the procedure 4 steps back, you will have to perform this step over and over. If you try to double or triple the amounts given, you may get more product, but you will hurt the yield.

dl-Lysergic acid. 3.9 g of the last product is mixed with 78 ml of 1.5% potassium hydroxide solution. Reflux for 30 min under nitrogen. 8.5 g of hydrogen sodium arsonate, and Raney Nickle (16 g wet), that has previously been deactivated by boiling in xylene suspension (see JOC, 455 (1948) to deactivate), is added and the mixture is refluxed and stirred under a nitrogen atmosphere for 20 hours. The solution is treated with carbon, and the crude lysergic acid is precipitated by neutralization to pH 5.6, and then filter it off and wash with water. Yield: 1.04 g. A second crop is obtained in the usual manner (0.15 g). Purify by dissolving in dilute ammonium hydroxide, treat with decolorizing carbon, and reprecipitate with carbon dioxide to get a mp of 242-243°. You may be able to get an analytical or laboratory consultant to make one of these products near the final step, thereby eliminating the need to go through all of the steps as described. This will save you much time, but as these people are highly trained, their time will be costly.

Lysergic acid can be made from many ergot derivatives by hydrolysis of these compounds. These compounds include ergonovine, ergotamine, ergokryptine, ergosine, methysergide, ergine, and a few others. Total synthesis of these compounds is impractical, as lysergic acid is made before the alkaloid. You could stop the operation as soon as you reach lysergic acid, otherwise you will have to hydrolyze as described below. There are many analogs of these alkaloids that end with the ine suffix. These are not as suspicious as the former because they lead to an inactive iso-LSD. They will look like this: the ergotamine isomer = ergotaminine, the ergonovine isomer = ergonovinine, etc. These analogs are easily converted to the active forms or they may be used exactly as the non-iso versions to give the iso-LSD, which is converted very easily to LSD as also described below.
Lysergic Acid From Ergot Alkaloids.

Dissolve 20 g of the alkaloid (use any of the above or one of its isomers or a combination) in 200 ml of 1 M methanolic KOH solution (this is made by dissolving 14 g of KOH in 250 ml of dry methanol) in a 1 1iter evaporation flask (heavy walled construction). Evaporate the methanol off. Add 400 ml of 8% aqueous (water) KOH solution to the residue and boil for one hour under a slow stream of nitrogen that is allowed to flow through a small orifice for exhausting purposes. Cool, acidify with dilute sulfuric acid, and shake in a separatory funnel with 1 1iter of dry ether. Separate the lower aqueous layer and filter it with vacuum assist. Wash the precipitate with 20 ml of dilute sulfuric acid. This is lysergic acid; store as described later in this chapter.

There remains a small amount of lysergic acid in the filtrate solution. Remove it by basifying the solution with sodium carbonate, and then bubbling CO2 through it. Filter it off and add it to the other lysergic acid. Now you will need to precipitate the iso-lysergic acid out and convert it. If you did not use any iso-alkaloid then you will have very little iso-lysergic acid, but it is still worth converting. If you used iso-alkaloid, this is a must.

Precipitate the iso-lysergic acid by adding some 10% HNO3, filter, add more portions until no more precipitate forms. Convert it to lysergic acid by adding 3 ml of 10% KOH per every 0.1 g of iso-lysergic acid, heat on steam bath for 1 hour under a nitrogen atmosphere. Precipitate the changed lysergic acid by acidifying with glacial acetic acid. The total yield of this entire operation (including the iso change) is a little under 10 grams. As stated earlier, you may use only iso-alkaloid in the hydrolysis step above to get iso-lysergic acid which can be used in the synthesis of LSD to get iso-LSD, which can be changed to the active LSD as described later. Note: iso-LSD is not active.

Some sources say that lysergic acid does not need to be purifed. I feel that everything should be purified. In the event that something should go wrong with the formula, you can immediately rule out impurities as the cause. Also, impurities create unwanted byproducts which can be poisonous, creating dangers for the drug user. Purification of lysergic acid is very easy. Dissolve the acid in dilute ammonium hydroxide, treat with decolorizing carbon, reprecipitate (after filtering off and washing product from the carbon) with carbon dioxide.

Convert iso-LSD to LSD. Add 50 ml of ethanol and 5 ml of 4 N KOH per every gram of iso-LSD. Let this mixture stand for 2 hours at room temp. Evaporate in vacuo to get the LSD.

Separate iso-LSD from LSD. Dissolve the residue of the mixture of LSDs from the end of the formula in 120 ml of benzene and 40 ml of chloroform. Add tartaric or maleic acid to precipitate the LSD, filter off, add a little ether and put in refrigerator for several days to get a little more LSD, which is filtered off and added to the rest. Evaporate the filtrate in vacuo to get the iso-LSD and convert as above.

LSD from Lysergic Acid. This is based on the formula taken from CA, 50, 10803d (1956) Dissolve 5.5 g of dry lysergic acid in 125 ml of acetonitrile that has been cooled to -10° and cool further to -20° with an external freezing mixture. Add 8.8 g of trifluoroacetic anhydride in 75 ml of acetonitrile (this solution must be cooled to -20° before the addition). Be careful making this addition, so as not to raise the temp, etc. Let stand at -20° until all the lysergic acid dissolves (about 1/2 hours). Add 7.6 g of diethylamine (or analog) in 150 ml of acetonitrile and allow to set at room temp in darkness for 2 hours. Evaporate in vacuo to get the LSD, which can be separated from the iso-LSD as above.

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Re: synthesizing LSD [Re: sam.larone]
    #9658460 - 01/22/09 11:58 AM (15 years, 2 months ago)

Synthesis of Lysergic Acid from Paspalic Acid

It is known that lysergic acid can be prepared by isomerizing paspalic acid, using potassium hydroxide2 or sodium hydroxide3, but these processes do not allow either good yields or a product comprising small quantities of isolysergic acid to be obtained industrially. A process has now been found, allowing lysergic acid of sufficient purity to be obtained in very good yields by isomerizing paspalic acid using a tetraalkylammonium hydroxide1, preferably tetrabutylammonium hydroxide. It is also possible to use the tetraalkylammonium hydroxide in a mixture with a small quantity of an alkali metal hydroxide, preferably sodium hydroxide.

The process is generally carried out in an inert solvent, such as water or a short-chain aliphatic alcohol (methanol or ethanol, for example), or in a mixture of these solvents, at a temperature preferably between 25-35°C, and then letting the reaction progress for 24 hours. The quantity of tetraalkylammonium hydroxide is generally from 1.5-10 mol and preferably 2.5 mol per mole of paspalic acid. When use is made of a mixture of tetraalkylammonium hydroxide and alkali metal hydroxide, the quantity of tetraalkylammonium hydroxide is generally from 0.5-2 mol, preferably 1.5 mol, and the quantity of alkali metal hydroxide is generally from 4.5-0.5 mol, preferably 1 mol, per mole of paspalic acid. Still more preferably, the process is carried out in an aqueous medium at a temperature of from 28-32°C., either in the presence of 2.5 mol of tetrabutylammonium hydroxide for one mole of paspalic acid or in the presence of 1.5 mol of tetrabutylammonium hydroxide and of 1 mol of sodium hydroxide for one mole of paspalic acid.

The lysergic acid is then precipitated by acidifying the reaction medium, using a mineral acid, preferably using sulphuric acid, and is filtered. It is advantageous to acidify to a pH of about 3-4, in particular to 3.5, while not exceeding 30°C.

Experimental
Example 11

130 g of paspalic acid are added rapidly to 780.1 g of a 40% strength solution of tetrabutylammonium hydroxide in water, with stirring and under a stream of nitrogen. The mixture is brought to 30±2°C. and allowed to react at this temperature for 20 hours. The reaction medium is cooled to about 20°C and held at this temperature for 3.5 h 918 g of water are added, followed by acidification using 95% strength sulphuric acid until the pH is 3.5, while maintaining the temperature at about 30°C. The reaction mixture is then cooled to 10±2°C. and held at this temperature for 30 minutes. The mixture is filtered through a sinter funnel under a vacuum of 0.4 bar, washed with 3x300 ml of water and then dried for 14 h at 75±2°C and 20 mbar. This gives 107 g of lysergic acid comprising less than 3% of isolysergic acid and the yield (weight/weight) is 80%.
Example 21

130 g of paspalic acid are added rapidly to 472.3 g of a 40% strength solution of tetrabutylammonium hydroxide in water, with stirring and under a stream of nitrogen, followed by 316 g of a 1.5N aqueous solution of sodium hydroxide. The mixture is brought to 30±2°C. and allowed to react at this temperature for 20 hours. The reaction medium is cooled to about 20°C. and held at this temperature for 3 h 30 min. 918 g of water are added, followed by acidification using 95% strength sulphuric acid until the pH is 3.5, while maintaining the temperature at about 30°C. The reaction mixture is then cooled to 10±2°C. and held at this temperature for 30 minutes. The mixture is filtered through a sinter funnel under a vacuum of 0.4 bar, washed with 3x300 ml of water and then dried for 14 hours at 75±2°C. and 20 mbar. This gives 107.8 g of lysergic acid comprising only 2.8% of isolysergic acid and the yield (w/w) is 81.6%.
Preparation of Lysergic Acid with Sodium Hydroxide Alone3

5g of paspalic acid in 100 ml of a 2N aqueous solution of sodium hydroxide are heated at reflux for 2 hours. After cooling, the pH of the reaction medium is brought to 5.5 by adding an aqueous solution of hydrochloric acid and glacial acetic acid (20 ml of water, 10 ml of HCl and 10 ml of acetic acid). The precipitate is filtered, washed with 3x20 ml of 50% aqueous methanol, then dried in vacuo at 75°C. This gives 3.15 g of lysergic acid comprising 6.8% of isolysergic acid and the yield (w/w) is 59.3%.
Preparation of Lysergic Acid with Potassium Hydroxide Alone2

5g of paspalic acid in 360 g of a 0.5N solution of KOH in a 50% aqueous ethanol is heated at reflux for 1 hour. After cooling, the pH of the reaction medium is brought to 5.5 by adding 1N HCl. The precipitate is filtered, washed with 3x20 ml 50% aqueous methanol, then dried in vacuo at 75°C. This gives 2.86 g of lysergic acid comprising 1% of isolysergic acid and the yield (w/w) is 49.8%.

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Re: synthesizing LSD [Re: sam.larone]
    #9658465 - 01/22/09 11:59 AM (15 years, 2 months ago)

Base-catalyzed Hydrolysis of Ergocristine to Lysergic Acid
by KrZ

Ergocristine base was obatined, and the subsequent base-catalyzed hydrolysis was a glowing success. The procedure here is very simple. Gloves should be worn at all times. Have a bucket of water to rinse the gloves in before you take them off so you will not contact the skin when trying to remove them, be careful cleaning all glassware.
Procedure

33.5g KOH was dissolved in 500ml dH2O in a 1000ml flask, and the solution was stirred magnetically, heating was commenced and the temperature of the solution was allowed to reach 75°C. 50g of Ergocristine base was added in 2g fractions over a period of 30 minutes. The mix went from clear to a light golden yellow tint over the course of the addition. Everything was in solution after 50 minutes. The reaction was allowed to proceed for a total of 5 hours after complete addition. Heating was removed and the reaction flask placed in a room temp. water bath, and then in an ice bath, until the solution was at 5°C. 325 mL 2.5 N H2SO4 was placed in an addition funnel, the flask placed in the ice-bath and stirred, and the acid was added dropwise. As the volume added reached ~200 mL pH metering was commenced, and addition was halted when the pH reached 3.0, ~50 mL of acid remained in the addition funnel. The flask was sprayed out with a stream of nitrogen, stoppered, wrapped in aluminum foil, and stored at 0°C for 18 hours (dark, of course). The flask was then removed, swirled vigorously to mix the solids, and quickly poured onto the buchner funnel. 100 mL of Et2O was added to the flask, in two fractions, swirled, and poured over the filter cake. The filter cake was placed in a vacuum dessicator in the dark for two hours. The filter cake was scraped into 500 mL NH3/EtOH solution, and the filter paper rinsed with two syringes full of the NH3/EtOH solution. The solution was stirred for 90 minutes (lights off), decanted, the solids re-extracted with a second 500 mL NH3/EtOH fraction (90 min. stirring, lights off), and filtered to remove the remaing solids (weight 1440 mg). The pooled extracts were stripped of solvent under vacuum at the rotovap (lights off, temp. set then left in dark). The solids remaing in the flask were taken up in 500 mL of 1% Aq. Ammonia. 250 mL 2.5 N H2SO4 was placed in the addition funnel, and added slowly with stirring to a beaker containing the extract. The pH was monitored continuously and addition was halted as the pH reached 3.0, the beaker was covered and placed in the refrigerator overnight. The solids were stirred vigorously to suspend them and collected by vacuum filtration. The beaker was swirled with 100 mL Et2O and the briefly suspended solids poured over the filter cake. The filter cake was placed in the vacuum dessicator for two hours (in the dark), and then weighed at 16.48g, placed in a brown glass vial, sprayed with nitrogen, sealed, wrapped in foil, and stored in the freezer at -10°C. The yield equates to 73%.

15% NH3 in EtOH prep.

1000 mL of 15% Ammonia in Anhydrous Ethanol was prepared by the slow addition of NaOH to cold absolute ethanol containg NH4Cl (not dissolved), filtration, and drying of the formed water by adding 0.20g CaO/1g H2O formed, with stirring and cooling. The formed calcium hydroxide was filtered.

Lighting

Regular lighting was used during the reaction. Two red photography lights were used during the rxn workup.

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Re: synthesizing LSD [Re: sam.larone]
    #9658475 - 01/22/09 12:01 PM (15 years, 2 months ago)

Hydrolysis of Ergotinine* to Lysergic Acid
Walter A. Jacobs & Lyman C. Craig
J. Biol. Chem. 104, 547-551 (1934)

The Ergot Alkaloids, Part II.
The Degradation of Ergotinine* with Alkali to Lysergic Acid

About 2 years ago, Smith and Timmis1 recorded the important observation of the formation of a basic degradation product, ergine, by the action of methyl alcoholic alkali on the ergot alkaloids, ergotinine and ergotoxine. From the analysis of ergine and a number of its salts, they derived for it the formula C17H21ON3. In the course of a systematic investigation of the effect of various hydrolytic procedures on ergotinine while confirming the formation of ergine by the procedure employed by Smith and Timmis, we have observed the formation in better yield of a new degradation product when aqueous alkali is used.

In preliminary experiments, it was found that crystalline ergotinine could be refluxed as a suspension in 6% aqueous KOH without appreciable alteration. This apparent resistance proved to be due to its insolubility. If ergotinine is first rapidly dissolved in methyl alcoholic potassium hydroxide and the solvent is immediately removed at low temperature and pressure, a resinous residue remains. When this residue is heated with aqueous alkali, as described later, it gradually dissolves with the liberation of ammonia due to cleavage of the amide group of ergotinine. Naturally, no ergotinine could be recovered from this reaction mixture. Furthermore, none of the base, ergine, could be detected on direct extraction of the alkaline hydrolysate. However, a new substance was obtained in good yield on gentle acidification, which possessed both acid and basic properties and which we have name lysergic acid. This acid is optically active (+40° in pyridine) and crystallizes in beautiful leaflets.

The analytical data obtained with the acid indicate a formula, C16H16O2N2. This is supported by the analysis of its methyl ester which was obtained with diazomethane. The acid has no methoxyl group but still possesses the original N- methyl group of ergotinine. Titration showed the presence of one carboxyl group. It still gives the characteristic blue Keller reaction of the original alkaloid.

The comparative accessibility of this degradation product in workable yield from ergotinine makes it an important object for further study. An attempt to determine its structure is therefore in progress.

The natural thought occurred that the failure to recover ergine from the above reaction mixture might have been due to the fact that although it could have been formed during the reaction in aqueous alkali it might have been further degraded to lysergic acid. In order to determine this point we have replaced ergotinine in the above procedure by ergine. Although a crystalline acid was obtained in small yield it appeared on analysis to be definitely different from lysergic acid. With the amount available it was possible to give it but preliminary study. A report of this work will be left to a later occasion.

When the above crude mother liquor from lysergic acid was continuously extracted with ether it was found that other acid material was formed in the reaction. From the ether extract, which smelled faintly of isobutyric acid, a crystalline ammonium salt was obtained which on analysis gave figures which approximated those of the salt of isobutyryl formic acid. This was definitely confirmed by its decomposition into isobutyric acid by the formation of the phenylhydrazone of isobutyryl formic acid.

Isobutyryl formamide was first obtained by Barger and Ewins2 by the destructive distillation of ergotinine. This experiment we have also repeated. The formation of isobutyryl formic acid itself, however, by what appears to be a hydrolytic cleavage under the influence of alkali may be significant. It is still premature however, to attempt to interpret its mode of linkage in the molecule. Although probable, it is not as yet certain that the amide group present in ergotinine itself is not the same as that which emerges as isobutyryl formamide on destructive distillation.

Note: Ergotinine is a 1:1:1 mixture of Ergocorninine, Ergocristinine and Ergocryptinine, and is isomeric with Ergotoxine, which is a 1:1:1 mixture of Ergocornine, Ergocristine and Ergocryptine (Ref: Merck Index XIII).

Experimental

1.0g of ergotinine was dissolved in 20ml of N-methyl alcoholic KOH and the methanol was removed at once by distillation at low pressure. The residue was treated with 20ml of an 8% aqueous solution of KOH and the mixture was heated on a steam-bath for 1 hour. A stream of nitrogen was passed through the flask during the heating and basic volatile material from the reaction mix was collected by passing the gas through a solution of dilute HCl acid.

After the reaction was completed, the HCl acid solution following evaporation gave a residue of 75mg which proved to be ammonium chloride. The theoretical weight for 1 mol of ammonium chloride is 88mg.

The alkaline solution was made acid to Congo red with sulfuric acid. At this point, a considerable amount of partly crystalline material precipitated. The acid suspension as such was placed in an extractor and exhaustively extracted with ether. This ether extract was worked up as given below for isobutyryl formic acid. The aqueous suspension which remained was then filtered. The dark colored solid was treated successively with 2x20ml portions of ammoniacal ethyl alcohol which left a residue which was inorganic. The filtrate on evaporation to dryness under reduced pressure gave a residue which was digested a short time with 5ml of methyl alcohol to remove colored impurities. After cooling, the undissolved crystals were collected. 0.26g of a slightly colored crystalline solid was obtained which melted with decomposition at 235°C.

Lysergic acid (although rather sparingly soluble) can be recrystallized best from water. It crystallizes as very thin hexagonal leaflets which melt with decomposition at 238°C. The melting point varies somewhat with the rate of heating. Repeated recrystallization failed to raise the MP. It separates with approximately 1mol of water of crystallization. This water is held very tenaciously and can be removed completely only on drying at 140°C/2mmHg. (+40° [c=0.500 in pyridine])

Lysergic acid gives the characteristic blue Keller test of the ergot alkaloids. In dilute sulfuric acid solution it gives with benzaldehyde and sulfuric acid a violet-blue ring which rises through the solution. With diazobenzensulfonic acid a brown amber color is given in carbonate solution. With alkaline nitroprusside a yellow is first formed, which gradually changes to a yellow-green.

Lysergic acid behaves both as an acid and a base. It is soluble in sodium hydroxide, ammonium hydroxide, sodium carbonate, and hydrochloric acid. It is but slightly soluble in dilute sulfuric acid. It is sparingly soluble in the usual neutral organic solvents but is quite soluble in pyridine.

On titration with alkali against phenolphthalein, the acid does not give a sharp end-point. However, the results indicated a neutralization equivalent of approximately 300 when the air-dried substance was used. Material dried at 140°C was not suitable for titration because of the appreciable discoloration which interfered with the detection of the end-point. 12.735 mg of substance were dissolved in 10m of hot water and the solution of titrated against phenolphthalein with 0.1N sodium hydroxide. Calculated for 1 eq., 0.489ml; found, 0.415 ml.
Lysergic Methyl Ester

Lysergic acid suspended in dry acetone slowly dissolved after the addition of diazomethane. The ester crystallized from benzene in thin leaflets which melted at 168°C. It is soluble in ether, acetone, alcohol, and hydrochloric acid. It is insoluble in ammonium hydroxide and petroleum ether.

The ethereal extract of the original acidified alkaline reaction mixture was dried with sodium sulfate and concentrated under reduced pressure. About 0.2g of an oil remained which smelled distinctly of isobutyric acid. It was completely soluble in water but not in petrolic ether.

A solution of the oil in 1ml of absolute alcohol was saturated with dry ammonia. On careful addition of ether crystals separated. After chilling the colorless material was collected. 50mg were obtained. It melted at 175°C with considerable sublimation before melting. A solution of the salt in 80% sulfuric acid, although odorless at first, developed a distinct odor of isobutyric acid on warming. The salt was analyzed as such without attempting recrystallization.

The analytical figures thus only approximated those required by the ammonium salt of isobutyryl formic acid and because of the limited amount of the material available the phenylhydrazone was prepared for characterization as follows: the ammonium salt was dissolved in 0.5ml of water and an equivalent of phenylhydrazine dissolved in 0.5ml of acetic acid was added. After a few minutes heating on the steam bath, the solution was carefully diluted. The phenylhydrazone crystallized on chilling. On recrystallization from dilute alcohol it formed long needles which melted at 152°C. This is higher than the figures given by Tschtschenke (128°C)3 and Tschelinzeff and Schmidt (143°C)4. Our substance was readily soluble in dilute ammonia and was reprecipitated in crystalline form on reacidification.

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Re: synthesizing LSD [Re: SheerTerror]
    #9658514 - 01/22/09 12:07 PM (15 years, 2 months ago)

So huge, not going to read all of that there.......some of those are just way to long.

We like Shulgin.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Re: synthesizing LSD [Re: TreeMoss]
    #9658605 - 01/22/09 12:22 PM (15 years, 2 months ago)

I like this one:

LSD-25
ACID; LYSERGIDE; D-LYSERGIC ACID DIETHYLAMIDE; METH-LAD; D-LYSERGAMIDE, N,N-DIETHYL; N,N-DIETHYL-D-LYSERGAMIDE; 9,10-DIDEHYDRO-N,N-DIETHYL-6-METHYLERGOLINE-8b-CARBOXAMIDE
 
SYNTHESIS : A solution of 6.7 g KOH in 100 mL H2O, under an inert atmosphere and magnetically stirred, was brought to 75 °C, and 10 g ergotamine tartrate (ET) added. The reaction mixture turned yellow as the ergotamine went into solution over the course of 1 h. The stirring was continued for an additional 3 h. The reaction mixture was cooled to about 10 °C with an external ice bath, and acidified to a pH of about 3.0 by the dropwise addition of 2.5 N H2SO4. White solids started to appear early in the neutralization; approximately 60 mL of sulfuric acid was required. The reaction mixture was cooled overnight, the solids removed by filtration, and the filter cake washed with 10 mL Et2O. The dry solids were transferred to a beaker, suspended in 50 mL 15 % ammonia in anhydrous ethanol, stirred for 1 h, and separated by decantation. This extraction was repeated, and the original decantation and the second extract combined and filtered to remove a few hundred milligrams of unwanted solids. The clear filtrate was stripped of solvent under vacuum, the residual solids dissolved in 50 mL of 1% aqueous ammonia, and this solution was acidified as before with 2.5 N H2SO4. The precipitated solids were removed by filtration and washed with Et2O until free of color. After drying under vacuum to a constant weight, there was obtained 3.5 g of d-lysergic acid hydrate, which should be stored in a dark, sealed container.

A suspension of 3.15 g d-lysergic acid hydrate and 7.1 g of diethylamine in 150 mL CHCl3 was brought to reflux with stirring. With the external heating removed, there was added 3.4 g POCl3 over the course of 2 min, at a rate sufficient to maintain refluxing conditions. The mixture was held at reflux for an additional 5 min, at which point everything had gone into solution. After returning to room temperature, the solution was added to 200 mL of 1 N NH4OH. The phases were separated, the organic phase dried over anhydrous MgSO4, filtered, and the solvent removed under vacuum. The residue was chromatographed over alumina with elution employing a 3:1 C6H6/CHCl3 mixture, and the collected fraction stripped of solvent under hard vacuum to a constant weight. This free-base solid can be recrystallized from benzene to give white crystals with a melting point of 87-92 °C. IR (in cm-1): 750, 776, 850, 937 and 996, with the carbonyl at 1631. The mass spectrum of the free base has a strong parent peak at mass 323, with sizable fragments at masses of 181, 196, 207 and 221.

This base was dissolved in warm, dry MeOH, using 4 mL per g of product. There was then added dry d-tartaric acid (0.232 g per g of LSD base), and the clear warm solution treated with Et2O dropwise until the cloudiness did not dispel on continued stirring. This opaqueness set to a fine crystalline suspension (this is achieved more quickly with seeding) and the solution allowed to crystallize overnight in the refrigerator. Ambient light should be severely restricted during these procedures. The product was removed by filtration, washed sparingly with cold methanol, with a cold 1:1 MeOH/Et2O mixture, and then dried to constant weight. The white crystalline product was lysergic acid diethylamide tartrate with two molecules of methanol of crystallization, with a mp of about 200 °C with decomposition, and weighed 3.11 g (66%). Repeated recrystallizations from methanol produced a product that became progressively less soluble, and eventually virtually insoluble, as the purity increased. A totally pure salt, when dry and when shaken in the dark, will emit small flashes of white light.

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Re: synthesizing LSD [Re: old mushmellow]
    #9658751 - 01/22/09 12:48 PM (15 years, 2 months ago)

Sounds like a nice Shroomery Gathering.  Surely there are some very connected people floating around somewhere.

Current or ex Intel operators?  Mafia?  Presidents?  War lords?

Aliens?

I'd say God but I heard that old son of a bitch keeled over.....after some shroomrites called him a homo.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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OfflinePoiesis
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Re: synthesizing LSD [Re: old mushmellow]
    #9658782 - 01/22/09 12:54 PM (15 years, 2 months ago)

Why did you bother to post all of those?  Do you think that you are proving your point by positng intimidating syntheses? 
You can say "either you are highly skilled chemists or you are stupid" but that is just a way of alienating those who would disagree with you.  You are trying to force an "us versus them" mentality instead of being reasonable.  It is not a fair way to argue and is not really an argument.  You are being silly and childish.
I would like you to explain where you get the $6000 figure.
I agree with johnm214.  Ultimately, the synthesis of LSD can be boiled down to a few steps involving boiling, refluxing and column chromatography.  If you want to argue that this is not the case then please make specific points.  Posting as many of the longest syntheses that you can find or just saying "either you agree with me or you are stupid" is a very childish way of trying to make a point.
Stamping your feet on the ground and screaming, "I am right and if you disagree then you are stupid!" is just going to cause people to lose interest in the thread.  I would like it if you could try actually discussing the topic like an adult.


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Re: synthesizing LSD [Re: Poiesis]
    #9658811 - 01/22/09 01:00 PM (15 years, 2 months ago)

Six grand would be about right if you made a "huge" amount and bought everything...........but I wouldn't make a huge amount myself or buy everything.

It would be great to make as much as you can from things you can get easily.......hell, a chemist really does have the advantage obviously but more to lose as well.  Unless he is a full time black market chemist.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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OfflinePoiesis
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Re: synthesizing LSD [Re: TreeMoss]
    #9658853 - 01/22/09 01:09 PM (15 years, 2 months ago)

He said $6000 for the lab equipment which is what johnm214 and I have asked him to explain.


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Re: synthesizing LSD [Re: TreeMoss]
    #9658869 - 01/22/09 01:12 PM (15 years, 2 months ago)

So, if we're talking about a small scale synth for personal use, what's a good estimate on supply costs? It'd be a rough guess of course, and not factoring in time or anything. What's a 'safely' cheap amount while not becoming ghetto, just sticking to the garage sale type of purchases? (eg. using some shitty container cause it's cheap even though the chemicals will eat it away over time.)

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Re: synthesizing LSD [Re: Poiesis]
    #9658871 - 01/22/09 01:12 PM (15 years, 2 months ago)

well hes got the right idea with having to do research before attempting a synthesis. John was saying you could easily do a synthesis and all the chemicals needed are readily available which is untrue. LSD is extremely rare in this country because of all the factors involved with making it.

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Re: synthesizing LSD [Re: Poiesis]
    #9658892 - 01/22/09 01:17 PM (15 years, 2 months ago)

lol, thanks Poiesis

Clearly he thinks I don't understand that crap he posted or don't know anything about chemistry

I refuse to get drawn into a discussion over knowledge or credentials cuz:
a) I'm not going to say who I am  anyways, and
b) I'm not going to give you info to verify it so you have no way of knowing anyways.
and finaly:
c)  Its all an appeal to authority and improper.  Someone who has no formal education can easily no more than a PhD.


I've done all the procedures mentioned so far in synthesises and purifications, and it doesn't matter.


Looking at the TIHKAL method, it would seem you could get away with:

1)  Air duster with nitrogen or other nitrogen source.
2)  Round bottom flask with appropriate necks
3) thermometer
4) condensor
5) filter flask
6)  Buchner funnel with filter
7) hot plate w/ stirrer
8) faucet aspirator (for solvent removal- add another erlenmeyer, stoper, and tubes/tubing for trap if you want)
9)  assorted other vessels for solvents and supernatant and shit shit plus something to hold the product and other crystals and whatever adapters or stoppers you need
EDIT: 10) Chromatography column with stationary phase


I'd want some TLC plates for the cafergot seperation and various qualitative analyses througout, but that's about it. 



All this shit can be bought new for 300$ or less- maybe 400$ with mostl new shit and a used or ebayed hot plate.


How

Edited by johnm214 (01/22/09 01:25 PM)

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OfflineTreeMoss
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Re: synthesizing LSD [Re: SheerTerror]
    #9658894 - 01/22/09 01:17 PM (15 years, 2 months ago)

Ya the amount of ET really isn't the issue as much as the vilotile things.  Those are watched and I wouldn't order from a chem supplier anyhow, maybe from overseas since customs isn't as concerned about some things like that coming through......if they even realized verses something coming from an in country supply company and the DEA reading the list with a fine tooth comb.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Re: synthesizing LSD [Re: SheerTerror]
    #9658909 - 01/22/09 01:20 PM (15 years, 2 months ago)

Quote:

SheerTerror said:
well hes got the right idea with having to do research before attempting a synthesis. John was saying you could easily do a synthesis and all the chemicals needed are readily available which is untrue. LSD is extremely rare in this country because of all the factors involved with making it.





I didn't say all the chemicals are readily available.  I just said I could do it and on microscale quantities it isn't that difficult (and I don't have any special source for lysergic acid/ergotamine)

I don't even have a degree or a chemistry job currently

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Re: synthesizing LSD [Re: johnm214]
    #9658955 - 01/22/09 01:29 PM (15 years, 2 months ago)

lysergic acid or ET is easy to get.......it's the diethylamine and some other thing..........but you can distill the diethylamine with ammonia and ethanol with some kind of chromo column or fractional distillation...not sure which would work........chem gurus?


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Re: synthesizing LSD [Re: SheerTerror]
    #9658961 - 01/22/09 01:30 PM (15 years, 2 months ago)

Krypto,
extracting crude alkaloids from C. purpurea might be the simplest way.  This involves a hotplate, a few flasks, alumina column, UV light, separatory funnel, and other common equipment.  Rigging a fume hood would be a good idea.  Handling ergot is no more dangerous than chemical reagents, so gloves, a lab coat and safety glasses are needed.  I estimate $500 - $1000 for the lab equipment.
The simplest synthesis does not involve exotic reagents, so maybe $200 - $500 for reagents.

SheerTerror, I did not see that Johnm214 said that all the chemicals are readily available.  By saying that the synthesis is easy, I think he was just trying to contradict the popular idea that LSD is the extraordinarily difficult synthesis it has been made out to be.  If you can read and understand the synthesis then it should be self-evident that synthesizing LSD is not "difficult."  I consider the difficultly to be relative to other chemical syntheses and not to tying shoelaces, of course.


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Re: synthesizing LSD [Re: Poiesis]
    #9658971 - 01/22/09 01:31 PM (15 years, 2 months ago)

YO! I didn't post all those. Only the easiest one. you're being obstinate poi. Just admit its not all "mix and stir". Refluxing is boiling NOOOOOB. Go take a ochem class then you and john can bitch slap me. I'm done with you foolish noobs.:kingcrankey:

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Re: synthesizing LSD [Re: Poiesis]
    #9658986 - 01/22/09 01:35 PM (15 years, 2 months ago)

Yeah, i didn't say it was all readily available, I said I could get the chemicals without extraordinary access (I know folks who use the more generic compounds that are harder to get, and I have access to all the stupid solvents and stuff).


Yeah, I was just breaking the myth that LSD is some exceptional synthesis.  Really its vocabulary.  Understand the terms and you can do it if you follow instructions.  The chromatography work is the most skilled portion- but I've done plenty of that and its just an experience thing- you can practice on other stuff with TLC plates.



All I was saying was that I could do a microscale synthesis without too much difficulty, and that anyone who had the stuff and was willing to read could as well without a whole lot of money.  I don't know anything about large scale stuff.

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Re: synthesizing LSD [Re: old mushmellow]
    #9658990 - 01/22/09 01:36 PM (15 years, 2 months ago)

What requires reflux with LSD?

Well, reflux is more than boiling it comes back unlike distillation.

But the thing about the ergot is that there are many alkaloids so how does it all turn into ET?  That doesn't make sense to me or how they are lysergic acid........it's a mystery for me.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Re: synthesizing LSD [Re: old mushmellow]
    #9658999 - 01/22/09 01:38 PM (15 years, 2 months ago)

Quote:

old mushmellow said:
YO! I didn't post all those. Only the easiest one. you're being obstinate poi. Just admit its not all "mix and stir". Refluxing is boiling NOOOOOB. Go take a ochem class then you and john can bitch slap me. I'm done with you foolish noobs.:kingcrankey:




thanks for the tip re: refluxing  I'll remember that.

Why would you bother re: ochem class?  If I said I'd taken one for a year  and scored so well on lecture and lab and then taken a more advanced specialized organic course and then some analytical courses and labs of relevance and then done a lil over two years of research work in organic chemistry you would have no reason to believe me anyways- would you?

Either address the argument or stop talking.  Personalisms don't prove your point.


And I know its not all mix and stir.  Its mix, stir, boil, pour, filter.  Tough shit.


Treemos:

No it isn't all ergotamine, that's why I said it would be easier to use cafergot for a microscale procedure. 

To purify mixed alkaloids you'd presumably do chromatography runs.  I've done many and you just kinda feel it out.  Use TLC plates and a GC if you have one to see what you're working with and try and seperate.


But in the end if you have a little bit of other alkaloids it probably won't matter too much.  No way to know of course, just guessing (which is bad habit).  You always have impurities.  Small amounts won't matter.  And when you use excess reagents you just react everything and the impurities likely aren't relevant at such small dosages.

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Re: synthesizing LSD [Re: TreeMoss]
    #9659005 - 01/22/09 01:39 PM (15 years, 2 months ago)

Quote:

TreeMoss said:
.it's the diethylamine and some other thing..........but you can distill the diethylamine with ammonia and ethanol with some kind of chromo column or fractional distillation...




You would have to look that up.  There is a way to make it and you are right, it involves distillation because you end up with ethylamine, dietylamine and triethylamine. 
The other reagent depends.  There is a method involving POCl3-DMF or one involving hydrazine.  Hydrazine can be made by doing what a bottle of bleach tells you not to do: mix bleach and ammonia.  There is more to it than that, but that is how it starts.
I think lysergic acid or ergotamine would be more difficult to find, at least as a pure starting material.

Scirus - for scientific information


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Re: synthesizing LSD [Re: old mushmellow]
    #9659018 - 01/22/09 01:41 PM (15 years, 2 months ago)

Quote:

old mushmellow said:
Refluxing is boiling NOOOOOB. Go take a ochem class then you and john can bitch slap me.




Refluxing is boiling under a condenser.
Who says I have not taken classes in organic chemistry before?  How would you possibly know that kind of thing?
I know it is not only mix and stir.  We are just saying that it is not difficult.
Insulting either of us and getting angry does not prove your point.  I think Johnm214 and I are actually interested in your point of view.  There is absolutely no reason for you to get upset.  If you made a point and were reasonable while making it, then I would address.  So far, you have been totally childish.


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Re: synthesizing LSD [Re: johnm214]
    #9659024 - 01/22/09 01:42 PM (15 years, 2 months ago)

alright well maybe it is something we should all be ambitious about trying

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Re: synthesizing LSD [Re: Poiesis]
    #9659025 - 01/22/09 01:42 PM (15 years, 2 months ago)

Ha, I didn't know hydrazine that was that simple as well....damn, this is looking good.

ET should be easy as finding it growing on some grass or wheat....really, especially fruiting it.

I never understood why a liquid culture is done.......I know it is quick and easy but I'd think the fruit yields more.......but not saying it's fact just thought.

I wish I could remember the book, but there are a few written back when LSD was becoming illegal about how to culture LSD and everything else...a real good read but not everything to satisfy you inquiring mind (as far as looking in every nook/cranny and dark corner goes).


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Re: synthesizing LSD [Re: TreeMoss]
    #9659047 - 01/22/09 01:47 PM (15 years, 2 months ago)

you don't need hydrazine for all procedures.  Like the tihkal one for instance.

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Re: synthesizing LSD [Re: johnm214]
    #9659057 - 01/22/09 01:48 PM (15 years, 2 months ago)

What is used in tihkal to replace then........didn't link that one together.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Re: synthesizing LSD [Re: TreeMoss]
    #9659090 - 01/22/09 01:54 PM (15 years, 2 months ago)

to answer you treemoss:
A suspension of 3.15 g d-lysergic acid hydrate and 7.1 g of diethylamine in 150 mL CHCl3 was brought to reflux with stirring.

You have to extract the assorted alkaloids and purify the D-lysergic acid.

No its not necessary to mess with poisons like hydrazine to accomplish the synth.

Ok poiesis how many grams of diethylamine do you need if you only have 2g of d-lysergic acid hydrate. Its on the test.

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Re: synthesizing LSD [Re: old mushmellow]
    #9659139 - 01/22/09 02:00 PM (15 years, 2 months ago)

Yep, I recall reading that line now.......didn't want to search for it and well.......reading is associated with the memory of mood and things like that.......I don't seem to isolate and store information like I would like.

So a chromo column to separate your lysergic acid?


and 4.5079 with a bunch of shit after that grams of diethylamine...guessing here....not double checked.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Re: synthesizing LSD [Re: johnm214]
    #9659179 - 01/22/09 02:06 PM (15 years, 2 months ago)

You might need equipment like this:



Appealing to authority.
I can say I have five PhDs if I want to.
How can anyone say it is true or not?
It does not matter anyway.


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Re: synthesizing LSD [Re: Poiesis]
    #9659188 - 01/22/09 02:08 PM (15 years, 2 months ago)

Gonna need more than a filtering set up.

And they are going to investigate your "educational" merits if they are really seriously believing anything other than a poke around on a non LSD manufacturing investigation.......as in not really an investigation as much as PO drop by or other knock n talk kind of thing...well, normally you don't let them in unless it's a PO and ya don't want them seeing anything funny.......they will take it and not give it back...just say it got lost or some shit.....they see you as a bug and them as God......


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Re: synthesizing LSD [Re: old mushmellow]
    #9659193 - 01/22/09 02:09 PM (15 years, 2 months ago)

And the answer is????????????????????????


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Re: synthesizing LSD [Re: old mushmellow]
    #9659211 - 01/22/09 02:12 PM (15 years, 2 months ago)

Quote:

old mushmellow said:
to answer you treemoss:
A suspension of 3.15 g d-lysergic acid hydrate and 7.1 g of diethylamine in 150 mL CHCl3 was brought to reflux with stirring.

You have to extract the assorted alkaloids and purify the D-lysergic acid.

No its not necessary to mess with poisons like hydrazine to accomplish the synth.

Ok poiesis how many grams of diethylamine do you need if you only have 2g of d-lysergic acid hydrate. Its on the test.





dude, seriously


We don't need a stoichiometry lesson.  This is gen chem stuff anyways.  How much diethylamine?  An excess.

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Re: synthesizing LSD [Re: johnm214]
    #9659236 - 01/22/09 02:15 PM (15 years, 2 months ago)

Well ya I want to know the number, if my math was the right method.

That and why reflux those two together......just to mix it all up or does it change......well ya it does......but why reflux, just good at it?


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Re: synthesizing LSD [Re: old mushmellow]
    #9659262 - 01/22/09 02:18 PM (15 years, 2 months ago)

You do not need to purify lysergic acid for all of the processes.  One way of doing it involves working with a crude mixture of ergot alkaloids.  You do not even need to start with any one particular alkaloid.
I am not going to pull out a calculator and convert molar ratios.  I believe you would use an excess of diethylamine anyway. 
I do not have all of the syntheses of LSD memorized and I am not going to pretend that I do.  I could open the PDFs and read them but I do not see any reason for that.
You were disagreeing about the difficulty of the LSD synthesis.  If you do not care to discuss that anymore then that is fine with me.  I am not going to take an online chemistry quiz just for you.


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Re: synthesizing LSD [Re: TreeMoss]
    #9659321 - 01/22/09 02:27 PM (15 years, 2 months ago)

It adds energy to the reaction and allows the molecules to combine more quickly. which they might not do otherwise.

Oh, c'mon poi take the quiz..Do it for yourself.

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Re: synthesizing LSD [Re: old mushmellow]
    #9659335 - 01/22/09 02:31 PM (15 years, 2 months ago)

So just heat for a catalyst and well, refluxing to keep it around.

I never understood it completely, I was visualizing a still but having the contaminates hang around and concentrate as well......but I guess you don't separate with a reflux and that was what I was figuring with cannabinoid refluxing....still a mystery there as well.....as that is the preferred way to make oil.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Re: synthesizing LSD [Re: TreeMoss]
    #9659369 - 01/22/09 02:38 PM (15 years, 2 months ago)

Yup, refluxing hash oil with a little H2SO4 causes isomerization of the delta THC analogues into the active. Then remove the solvent en-vacuo or distill.

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Re: synthesizing LSD [Re: old mushmellow]
    #9659381 - 01/22/09 02:41 PM (15 years, 2 months ago)

Sweet, in a few years I'd like to get a still and have been shopping for one with a funnel attachment......for making ETHER.

A little scared to make that, any tips?

I haven't shopped for a reflux, that would be after a still.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Re: synthesizing LSD [Re: TreeMoss]
    #9659407 - 01/22/09 02:46 PM (15 years, 2 months ago)

Can't you just buy ether?


--------------------
I know... that just the smallest
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Re: synthesizing LSD [Re: zouden]
    #9659415 - 01/22/09 02:48 PM (15 years, 2 months ago)

No I cannot without paranoia, I wouldn't want to explain why or risk having someone being an asshole about it.....but cops would rather see me on fire so hey.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Re: synthesizing LSD [Re: zouden]
    #9659431 - 01/22/09 02:51 PM (15 years, 2 months ago)

You can only buy Diethyl Ether and Petroleum Ether

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Offlinezouden
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Re: synthesizing LSD [Re: SheerTerror]
    #9659447 - 01/22/09 02:54 PM (15 years, 2 months ago)

Yes. What else is there?


--------------------
I know... that just the smallest
                                                part of the world belongs to me
You know... I'm not a blind man
                                                    but truth is the hardest thing to see

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OfflineTreeMoss
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Re: synthesizing LSD [Re: SheerTerror]
    #9659473 - 01/22/09 02:58 PM (15 years, 2 months ago)

Quote:

SheerTerror said:
You can only buy Diethyl Ether and Petroleum Ether




What do you mean by that?  I wouldn't want to buy ether it raises eyebrows in a way I wouldn't want anything to come of it....but then again buying a grow light used to make me nervous.

then again, so did cigs and beer at one time.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Invisibleold mushmellow
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Re: synthesizing LSD [Re: TreeMoss]
    #9659492 - 01/22/09 03:00 PM (15 years, 2 months ago)

Heat a pure ethyl alcohol with conc. H2SO4 to 140c will lead (produce) to diethyl ether. the hydrogen byproduct is explosive. Just buy it. I wouldn't worry about that chem.

Petroleum ether is an alkane not a real ether.

Edited by old mushmellow (01/22/09 03:22 PM)

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OfflineTreeMoss
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Re: synthesizing LSD [Re: old mushmellow]
    #9659534 - 01/22/09 03:08 PM (15 years, 2 months ago)

I never read about lead being involved........and the hydrogen? 

I read about peroxides that can form when it is exposed to things such as light, air or metal.......but that copper could prevent that during storage.


--------------------
Drug chemicals are going to be more abundant and survive longer than any anti-drug agendas.  Some of us are just ahead of the game, we already know what the future will understand.  Drugs weren't bad but how some people used them were and some people just were bad because they had to be.

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Offlinezouden
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Re: synthesizing LSD [Re: old mushmellow]
    #9659561 - 01/22/09 03:12 PM (15 years, 2 months ago)

I tried sniffing ether once (I have lots at work). It was... boring.


--------------------
I know... that just the smallest
                                                part of the world belongs to me
You know... I'm not a blind man
                                                    but truth is the hardest thing to see

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Invisibleold mushmellow
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Re: synthesizing LSD [Re: zouden]
    #9659631 - 01/22/09 03:25 PM (15 years, 2 months ago)

:rofl2::toast:

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OfflineSheerTerror
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Re: synthesizing LSD [Re: zouden]
    #9659675 - 01/22/09 03:33 PM (15 years, 2 months ago)

yea i havent heard anything good about it

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OfflineRazoom
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Re: synthesizing LSD [Re: SheerTerror]
    #9750567 - 02/06/09 04:06 PM (15 years, 2 months ago)

The large mushrooms, however - give more various on action from their, and colourful visual space.
Do not overlook(forget) that LSD from a mushroom. Can there is an active substance some more best sincere quality?

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OfflineSeussA
Error: divide byzero


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Re: synthesizing LSD [Re: Razoom]
    #9750824 - 02/06/09 04:34 PM (15 years, 2 months ago)

Quote:

he large mushrooms, however - give more various on action from their, and colourful visual space.
Do not overlook(forget) that LSD from a mushroom. Can there is an active substance some more best sincere quality?




Be what said he yes understand maybe no big big whee!


--------------------
Just another spore in the wind.

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OfflineRuNE
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Re: synthesizing LSD [Re: Seuss]
    #9750991 - 02/06/09 04:54 PM (15 years, 2 months ago)

:lol:


--------------------
~Happy sailing~

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OfflineRazoom
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Re: synthesizing LSD [Re: RuNE]
    #9751133 - 02/06/09 05:13 PM (15 years, 2 months ago)

In English there would be no words what to receive worthy translation from that language on which I speak.  :yoda2:

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OfflineSeussA
Error: divide byzero


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Re: synthesizing LSD [Re: Razoom]
    #9751174 - 02/06/09 05:19 PM (15 years, 2 months ago)

> In English there would be no words what to receive worthy translation from that language on which I speak.

And yet you tried to put into English that which cannot be translated.  Ponderous.

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OfflineRazoom
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Re: synthesizing LSD [Re: Seuss]
    #9751239 - 02/06/09 05:29 PM (15 years, 2 months ago)

You tried to take for example Baeocystin from a mushroom?
I speak about that that some mushrooms absolutely differently work. I think that by a simple explanation, greater percent(interest) of known substance, here to not do without.

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