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Mushrooms, Mycology and Psychedelics > Advanced Mycology
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Re: mushroom extraction - psilocybin hcl salt [Re: JssMthrFcknChrst]
    #1258111 -

Quote:
No doubt Hofmann knows his shit, but we don't, and want to keep it as simple as possible.


...but you can't expect the process of extracting pure crystals of psilocybin to be simple. Crude extractions have been posted and those are effective but they are crude.


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"A celibate clergy is an especially good idea, because it tends to suppress any hereditary propensity toward fanaticism." - Carl Sagan

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Re: mushroom extraction - psilocybin hcl salt [Re: the spiral]
    #1258481 -

We're aiming for a trade off - decent purity for ease of process. Pure would be awesome, but at least for the early trials, simplicity and cost win out. If we find that this process creates unacceptable product, we will undoubtably move on to something more complex. Thanks for the suggestions, and we will be coming back to this at some later time, even if just for experimentation.

jssmthrfcknchrst


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Re: mushroom extraction - psilocybin hcl salt [Re: X.O]
    #1261355 -

Any one think that a pre-washing the powered mushrooms with acetone then extracting with methanol, and finally washing the crystals with acetone again would be a good approach?

I figure the prewash will help keep the extract solution clean, even before it has extracted... Since acetone is a flop for extracting the alkaloids, it shouldn't affect the yield.

Can anyone see a problem with this?

PS - found acetone at a well known Mart chain, Kleen Strip Acetone. Label claims 100% pure. Less then $3 a quart!


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Post deleted by Moe Howard [Re: JssMthrFcknChrst]
    #1261562 -



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I'm a huge idiot

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Re: mushroom extraction - psilocybin hcl salt [Re: X.O]
    #1261580 -

point taken. still, i doubt the purity of the crystals that the simpler methods produce. considering that i have never attempted any of these techniques, however, i'm hardly an authority!


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"A celibate clergy is an especially good idea, because it tends to suppress any hereditary propensity toward fanaticism." - Carl Sagan

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Re: mushroom extraction - psilocybin hcl salt [Re: JssMthrFcknChrst]
    #1263174 -

Be very careful with lye. OTC NaOH contains high levels of heavy metals. Mercury, Lead, ect. Very Bad stuff.

You are definately not going to be able to use an OTC non polar solvent. Ether are something will work. A Cl based solvent would be better. Good luck getting the stuff and be careful (they are watching out for the meth kiddies). But you are going to need a vacuum distallation setup to get an acceptable solvent.

Psilocybin is known for being extremelly unstable and is found in very small quanities. Crystalizing it, then separating such a small amount is quite an undertaking.

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Re: mushroom extraction - psilocybin hcl salt [Re: vader]
    #1270390 -

The document on this website explaining how to grow mycelium on agar cultures states that an a/b extraction will not work on psilocybin. That it will dissolve in both polar and non-polar solvents. And whats wrong with vader. I think hes just talking out his ass. You don't need ether you can use otc non-polars for an a/b. And no ones going to think your making meth unless you buy everything at one store at the same time. And why do you say psilocybin is extremely unstable?? I think your thinking of lsd. If an a/b does work on psilocybin most people will be able to perform it. Its not hard at all to do an a/b extraction. Vader can't even spell so no one listen to his bullshit!! He's full of himself. otc solvents are pure enough for this type of thing. And no one has mentioned gassing with hcl to recover the psilocybin hcl from the non-polar. No evaporation is needed with gassing so theres no heat that can possible harm the chemical. Then just wash with acetone and recrystillize in acetone. Thats how i'd do it.

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Re: mushroom extraction - psilocybin hcl salt [Re: Teragon]
    #1271193 -

Does anyone have any idea how much impact the pre-wash with acetone will have on the final yield?

Thanks!

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Re: mushroom extraction - psilocybin hcl salt [Re: Dr. Slavic]
    #1274195 -

Ten points for dr. Slavic! Indeed, psilocybin can not be isolated by means of a classic acid/base extraction as described by X.O.

That is because psilocybin is a internal salt (due to the phosphoryloxy group). Even the freebase version of the molecule is polar, so it will never move to the naphta layer when the lye is added to the water extract. Only psilocin, 4-OH-n-methyltryptamine and 4-OH-tryptamine can be isolated in this style but they are very minor components of the mushrooms and very unstable. Especially in alkaline environments (the lye will destroy them).

For psilocybin there may be no other option than using alcohol. Methanol is best, but a mix of water and ethanol (=vodka) works too, especially if you use a lot of it and several soaking periods of a few hours each. Psilocybin doesn't dissolve readily in pure ethanol but it does very well in water. 140 proof alcohol is fine. No problem if it is denatured with methanol or acetone (as long as you do not drink it of course).

Unfortunately, for most alkaloids mixed phase extractions are far less specific than acid-base extractions. The result is usually not crystals but an oil.

The oil then needs to be purified, for instance by means of chromatography. I am afraid that is also the case with psilocybin. The method in the link in the beginning of this thread works. But unfortunately the crystals which do form are mainly urea, and the total residue is not purer than 30 percent psilly. Urea is also an alkaloid. It is not really toxic but not psychoactive either. Psilocybe mushrooms may contain three times more urea than psilly.

I have tried to dissolve the crude brown extract in boiling ethanol. It certainly cleaned it up a bit but not to nice white-transparent crystals. Same with toluene, diethyl ether and petroleum ether. The dark residue only dissolves readily in water.

Perhaps that the residue can be further purified when it is dissolved in a boiling mixture of ... parts of acetone (in which psilocybin does not dissolve) and ... parts of distilled water (in which it readily dissolves). When this mixture is slowly cooled there should be a moment that the psilocybin crystallizes out and the unwanted gunk stays in solution. Or the other way around. It is possible that for a nice endproduct the mixture needs to be of a certain pH and/or saturated with a specific salt. Etcetera etcetera.

See why mixed phase recipes are so difficult to compose? There are too many factors for beginning students like me!

Fortunately, chromatography always works. But you need specialized types of paper, developer liquids and color reagens for that.

For now the needed mixed phase recipe is still a big puzzle. You will need tons of mushrooms to find it by guessing&testing - or a lot of luck!

The good news howver is that once the recipe is there it is easy. Just a mixture of OTC liquids. So in case that a lucky person reads this thread - feel free to post the recipe!

Yachaj

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Re: mushroom extraction - psilocybin hcl salt [Re: mycophreak]
    #1278084 -

If I remember my chemistry right, almost any HCl salt will be insoluble in acetone. After the "dirty" solid has been obtained from washing in methanol, one could use acetone to remove the "gunk" from the solid, leaving a more pure HCl salt.

However, anhydrous acetone should be used to avoid losing the any of the salt. If their is water in the acetone, some of the salt will dissolve and be washed away with the acetone.


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Should the US relegalize drugs?

http://www.lp.org/issues/relegalize.html

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Re: mushroom extraction - psilocybin hcl salt [Re: BigJohnson]
    #1280899 -

When some one does get a pure form from the extract please try his for me. Snort some just for the hell of it. Just some thing I've wanted to try for some time now. Oh yeah and put a post up about it.


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A simple opinon from another monkey with a voice.

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Re: mushroom extraction - psilocybin hcl salt [Re: Sacik]
    #1283022 -

why are all of X.O.'s post gone??


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work of fiction

http://www.thenook.org/

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Re: mushroom extraction - psilocybin hcl salt [Re: JssMthrFcknChrst]
    #1283043 -

after washing with acetone, could the water soluble psilo be washed with water and then evap the water to clean the acetone off?
This sounds much easier than a RP/I extract of of meth from E. Im definately going to experiment.


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Edited by Audi0 (02/05/03 06:53 PM)

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Re: mushroom extraction - psilocybin hcl salt [Re: IDontGrow]
    #1283410 -

I second that. Why are X.O.s interesting contributions removed? sHe is a Shroomery administrator, which means that it must be a very educated person from who we can learn. That is why I am here. And I remember that sHe posted a very detailed psilly isolation technique. The text wasn't hypothetical at all - it was clearly written in a style which suggested that X.O had tested it him/herself.

No need to remove the text simply because I disagree with it. Science can only develop in an uncensored environment of free speech/discussion. Do not take me that serious. Like I wrote, I am just a student and X.O is a shroomery ADMINISTRATOR.

Anyway, the acetone doesn't help much in the end IMHO. The filtered 140 proof alcohol extract is brought at a pH3 with a drop of muriatic acid (supermarket grade), evaporated down, defatted with naphta and then the acetone is added. Yellowish toplayer = removed and more acetone added. Now the toplayer stays clear. On the bottom is mysterious dark matter. I have heard it can produce galaxies and that it is about 30 times as potent as semilanceata. But further purification (maximum will be about 100 times as potent as semilanceata) will be difficult without chromatography. At least that is what I think. Ask expert X.O. for a tested method which works.

Yachaj

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Re: mushroom extraction - psilocybin hcl salt [Re: mycophreak]
    #1283429 -

XO is NOT a shroomery admin LoL he just put that under his name. He is an OTD tard and prolly got his ass banned or something.


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Re: mushroom extraction - psilocybin hcl salt [Re: mycophreak]
    #1283592 -

Hey. That is weird. The mysterious dark matter doesn't dissolve in 192 proof ethanol at roomtemperature.

But if the dark matter is loaded in a 30ml bottle (miniature hard liquor bottle) along with 10ml of 192 proof alcohol (denatured with acetone for cheapness), firmly closed, boiled in a pc (do not choose a thin walled bottle for this!) and slowly cooled to roomtemperature, after which the liquid is poured in a 2nd bottle, then the molten but not-dissolved dark matter remains in the 1st bottle. But the alcohol in the 2nd bottle becomes milky white when the temperature is minus 20 centigrade. The milkyness stays if the bottle is returned to roomtemperature, and seems to be caused by tiny white crystals which are insoluble in acetone, ethanol, naphta and toluene but which are very soluble in water (water is the only solvent which stays transparent when the powder is added - the rest stays milky). The crystals precipitate on the bottom of the 2nd bottle.

When a few ml of the milky white ethanol is evaporated in a shallow dish, and one drop of freshly prepared Marquis reagent (=45 volume parts (drops) of 37 percent sulphuric acid plus 1 volume part (drop) of 37 percent formaldehyde) is added to the crystals, an orange color reaction develops in about 5 minutes.

Strange. Does any one of you have a clue what this white powder can be?

Yachaj

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Re: mushroom extraction - psilocybin hcl salt [Re: IDontGrow]
    #1284602 -

It happened to me too. A little bit back, when the webstie changed, some names were deleted and all posts by them disappeared. I had to re-register my name, and if I search for posts by the old me, it finds nothing.


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Re: mushroom extraction - psilocybin hcl salt [Re: mycophreak]
    #1296164 -

Quote:
That is because psilocybin is a internal salt (due to the phosphoryloxy group). Even the freebase version of the molecule is polar, so it will never move to the naphta layer when the lye is added to the water extract.


So this means that naphtha can be used to defat the solution, right? I imagine that a methanol extraction, washed a few times with naptha, acetone, ether, chloroform, and DCM, then evaporated might yield a rather pure endproduct. Is psilocybin soluble in any of these solvents? Would any of them react with each other?


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"A celibate clergy is an especially good idea, because it tends to suppress any hereditary propensity toward fanaticism." - Carl Sagan

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Re: mushroom extraction - psilocybin hcl salt [Re: the spiral]
    #1296801 -

One washing with acetone should do the trick, assuming it was filtered while dissolved in your alcohol.


--------------------
Should the US relegalize drugs?

http://www.lp.org/issues/relegalize.html

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Re: mushroom extraction - psilocybin hcl salt [Re: mycophreak]
    #1296852 -

Anyone know a good method of drying acetone? I've read about using epsom salts from the grocery store, but i dont think i quite understand the process.

thanx


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