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JohnRainy
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Psilocin extraction internet recipe
#26385457 - 12/16/19 04:28 PM (4 years, 2 months ago) |
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Im going to try this in the nearish future.
Quote:
A representative sample of 2 to 10g of dried mushrooms is ground to a fine powder by mortar and pestle. The powder is mixed with 100 mL of dilute acetic acid in a 250-mL beaker. The pH is readjusted to pH 4 with glacial acetic acid. After standing 1 h, the beaker is placed in a boiling water bath for 8 to 10 min or until the internal temperature of the acid mixture reaches 70°C. The beaker is removed and cooled to room temperature under running water. The acid mixture is separated from the mushroom powder by suction filtration using glass wool. The filtrate is brought to pH 8 with concentrated ammonium hydroxide and quickly extracted with two 50-mL portions of diethyl ether. Gentle mixing instead of shaking should be used to prevent an emulsion. The ether is dried over sodium sulfate, filtered, and evaporated under nitrogen with no applied heat. Crude psilocin will appear as a greenish residue. Recrystallization from chloroform/heptane (1:3) yields white crystals. The resulting powder can then be submitted to infrared and mass spectral analyses.
I got to thinking about the process, and am wondering if it might be more convenient to use a vacuum chamber to evaporate the acetic acid solution, then add the diethyl ether to bring the psilocin into it and separate it from the acetic acid, pour off the solution to separate it from the acetic acid which I assume will not dissolve in the diethyl ether, and then evaporating the diethyl ether/psilocin solution in the vacuum chamber, hopefully running the vacuum pump's output through a condenser so I can save the diethyl ether and reuse it.
That way I wouldn't need to evaporate it under nitrogen or use sodium sulphate to dry the diethyl ether solution, hopefully.
Final step would be to open the vacuum chamber and quickly pour in liquid honey, or vodka, or whatever medium to put the psilocin into a consumable form where it won't oxidize.
Maybe Im way off. Anyone here a chemist?
Edited by JohnRainy (12/16/19 04:36 PM)
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rido



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Re: Psilocin extraction internet recipe [Re: JohnRainy]
#26385466 - 12/16/19 04:37 PM (4 years, 2 months ago) |
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I'd recommend trying the process as written before trying it with any major changes unless you're an experienced chemist, then of course use your knowledge and experience to make improvements.
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StygianKnight
A Mushroom

Registered: 03/12/12
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Re: Psilocin extraction internet recipe [Re: rido]
#26385546 - 12/16/19 05:32 PM (4 years, 2 months ago) |
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I see two issues.
One is that this is to convert the stable psilocybin into less stable psilocin for sample testing, and if you can you want to keep that phosphate group for stability.
Two, glacial acetic acid isn’t something you want to mess with without proper ventilation and safety gear. It’s anhydrous acetic acid and is rather pungent.
It is indeed possible to extract and even crystalize psilocybin but it’s a pain in the ass and takes a bit of chem experience and equipment to do. Which is why it’s so rarely seen.
When looking at any other extraction technique that contains water, one of the first steps you should do is to make sure your shrooms have been dried hot and all the dephosphorelating enzymes have been destroyed.
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Digit
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Re: Psilocin extraction internet recipe [Re: StygianKnight]
#26385756 - 12/16/19 06:58 PM (4 years, 2 months ago) |
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I'm pretty sure that the point of extracting with an acid and then raising the pH to 8with ammonia is to liberate the psilocin as the free base so it will be soluble in the ether. If you just evaporate the acetic acid, (which will stink like hell and make your neighbors wonder if you're operating a clandestine pickle factory), the residue left after you evap the acid will contain a water soluble form of psilocin that will not dissolve in ether. The reason why no one (outside of the legit scientific community) bothers extracting psilocybin/psilocin from mushrooms is because it's difficult, highly inefficient and a waste of time. Just make tea, or grind your mushies and capsule them if you hate the taste.
-------------------- Question everything. Believe nothing. Think for yours3lf.
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JohnRainy
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Re: Psilocin extraction internet recipe [Re: Digit]
#26385789 - 12/16/19 07:12 PM (4 years, 2 months ago) |
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Is 150-160F hot enough to destroy the dephosphorelating enzymes?
Did a little reading on acetic acid. I wasn't expecting there to be much issue with it since I eat it all the time, but there is.
Quote:
This liquid is highly corrosive to the skin and eyes and, because of this, must be handled with extreme care. Acetic acid can also be damaging to the internal organs if ingested or in the case of vapor inhalation.
Im confident I can work with it safely despite this. Ill wear my goggles. The container of it would only be open for brief periods.
Extraction is rarely done. Ive never seen it. Seems like it would be really boss to have some nice purified magic.
Im not interested in the recrystallization. Was going to skip that part.
If this process produces freebase psilocin, that means it is no longer active via the stomach but rather must be smoked, right?
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spiritlands



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Re: Psilocin extraction internet recipe [Re: JohnRainy]
#26386139 - 12/16/19 10:17 PM (4 years, 2 months ago) |
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Acetic acid actually does mix with ether. It has the property of being able to mix with polar and non polar solvents. The byproduct of bringing the pH to 8 is ammonium acetate which is very hydrophilic and stays behind in the water as a salt. The acid and the ammonia should cancel each other out leaving water and salt so there shouldn't really be any acid by the time you hit it with ether. The ether will bond to a small percentage of the water from the reaction. It's called an azetrope. I believe it retains 6% water due to hydrogen bonding that's why the step of drying it with sodium sulfate. With ether you could substitute other desiccants as long as they dissolve in water and not ether. If this part is skipped it won't crystalize. I believe that's why they do it the way they did. I'm glad there's some interest in it. I'll be trying it to this weekend. Have a cube flush coming in right now to try it on.
Oh and household distilled white vinegar has a pH around 2.5, were only going to 4. Acetic acid isn't that big of a deal unless your huffing it and rubbing your eyes with it. It stings the eyes and nose more than it burns the skin.
Since it only needs to go up 1.5 pH this can prob be done by freezing it and collecting the slushy part. Then pH test it and dilute it back down to 4. I'll freeze some tonight and pH it in the morning so we know how much it concentrates it. I've done something similar in the past but it doesn't freeze like ice it stays like a melty slushy but we don't need ALL the water out just some.
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JohnRainy
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Re: Psilocin extraction internet recipe [Re: spiritlands]
#26386205 - 12/16/19 11:34 PM (4 years, 2 months ago) |
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Thank you for that clarification.
Do I understand it right to say that the concentrated ammonium hydroxide chemically transforms the acetic acid out of existence leaving ammonium hydroxide which stays behind in the water after the diethyl ether extraction?
Quote:
CH3COOH + NH. H2O → CH3COONH4 + H2O. Acetic acid react with ammonium hydroxide to produce ammonium acetate and water. Acetic acid - concentrated solution.
I think I just answered my own question. Thanks internet.
What do you think about evaporating the diethyl ether/psilocin solution in a vacuum chamber rather than in a nitrogen atmosphere?
Sounds like I can skip the desiccant too. I don't care to do recrystallization.
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spiritlands



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Re: Psilocin extraction internet recipe [Re: JohnRainy]
#26386223 - 12/17/19 12:12 AM (4 years, 2 months ago) |
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That's my plan. Vacuum chamber. I will do the crystallization just to say I did it. The problem is good ether sources are typically starting fluid for over the counter. It is a mix of hexane/heptane water and diethyl ether. Depending on brand. All them are somewhat dissolved in each other. They do this bc ether is unstable. It has such high hydrogen bonding when it's pure that it can generate enough static electricity to donate itself. It burns at a rate twice as fast as dynomite. This is part of why I prefer vacuum distillation. Usually I don't mind heptane in the mix but in this case I do bc heptane takes one eternity to evap and it leaves oily residue. So I'm thinking up a way around this. And chloroform isn't readily available but can be made. I'm thinking toluene, or dichloromethane. Those are both otc and much safer.
Tomorrow I'll share how I build my aspirator using a 'T' fitting, rtv and a ball point pen. And I'll show the setup and operation. We'll get through this together and learn some shit in the process.
Edited by spiritlands (12/17/19 12:47 AM)
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JohnRainy
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Re: Psilocin extraction internet recipe [Re: spiritlands]
#26386237 - 12/17/19 12:36 AM (4 years, 2 months ago) |
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Edited by JohnRainy (12/17/19 12:43 AM)
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spiritlands



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Re: Psilocin extraction internet recipe [Re: JohnRainy]
#26386248 - 12/17/19 12:53 AM (4 years, 2 months ago) |
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Damn that's sweet. That used to be hard to get. Ya that would be ideal. With precaution. No evaporating inside. I think toluene is a cheaper safer choice though.
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YogiBear



Registered: 08/24/19
Posts: 845
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Re: Psilocin extraction internet recipe [Re: JohnRainy]
#26386257 - 12/17/19 12:57 AM (4 years, 2 months ago) |
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I use to be on the DMT Nexus and that does look like a biochemist TEK for sure.
Im just grinding them up in chochlates and work fine.
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JohnRainy
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Re: Psilocin extraction internet recipe [Re: spiritlands]
#26386267 - 12/17/19 01:02 AM (4 years, 2 months ago) |
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Is this acceptable?
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JohnRainy
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Re: Psilocin extraction internet recipe [Re: YogiBear]
#26386273 - 12/17/19 01:08 AM (4 years, 2 months ago) |
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This doesn't sound that hard to pull off, does it? You need a few things, and you have to be careful not to spill the toluene, but we're talking about pure psilocin here.
That would be so boss.
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YogiBear



Registered: 08/24/19
Posts: 845
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Re: Psilocin extraction internet recipe [Re: JohnRainy]
#26386307 - 12/17/19 01:36 AM (4 years, 2 months ago) |
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Would definately be nice for dosing accuracy 👍
Learning how the chemical you want drifts back and forth based on ph is a pretty awesome concept to work with.
Have done mesculine extractions too. This sounds more like that but used Toulene for dmt only so I dont understand how psilocilo works as a chemical
Good luck and keep us posted
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spiritlands



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Re: Psilocin extraction internet recipe [Re: JohnRainy]
#26386311 - 12/17/19 01:41 AM (4 years, 2 months ago) |
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That's the stuff. My fav solvent. I don't think it will be hard at all but it's different reading it than it will be too do it. Couple of tries to figure out the fun parts and it should be pretty simple. I'm digging through my garage right now looking for my merk index. It's a book every aspiring chemist should own. It is a giant book of chemicals and their properties, patent numbers, synthesis etc.
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JohnRainy
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Re: Psilocin extraction internet recipe [Re: spiritlands]
#26386322 - 12/17/19 01:48 AM (4 years, 2 months ago) |
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I don't understand shit about this.
https://people.chem.umass.edu/xray/solvent.html
It's properties of solvents. In the results and discussions, the extraction method authors mentioned something about their process being very good for isolating psilocin from other methanol soluble compounds. Can toluene do this as effectively as well?
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YogiBear



Registered: 08/24/19
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Re: Psilocin extraction internet recipe [Re: JohnRainy] 1
#26386357 - 12/17/19 02:34 AM (4 years, 2 months ago) |
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I think you should join the dmt nexus brother. They will have your answers for You
Its all about the composition of the molocule you are extracting as to which solvent to use and what PH it need to be to get it to drift from one solution to another
Not many people here are going to be able to get you where you want to go
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sh4d0ws
LSx


Registered: 02/26/08
Posts: 12,086
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Re: Psilocin extraction internet recipe [Re: JohnRainy]
#26386393 - 12/17/19 03:17 AM (4 years, 2 months ago) |
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Quote:
JohnRainy said: What about this?
https://www.amazon.com/s?k=diethylether&ref=nb_sb_noss_1
Anybody wanna try some ether? 
Quote:
February 28, 2019 Verified Purchase Hunter S Tompson was a huge fan I'm an not hahaha 14 people found this helpful
Fucking amazon eh!!!!
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sh4d0ws
LSx


Registered: 02/26/08
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Re: Psilocin extraction internet recipe [Re: YogiBear]
#26386395 - 12/17/19 03:20 AM (4 years, 2 months ago) |
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Quote:
YogiBear said: I think you should join the dmt nexus brother. They will have your answers for You
Its all about the composition of the molocule you are extracting as to which solvent to use and what PH it need to be to get it to drift from one solution to another
Not many people here are going to be able to get you where you want to go
DMT-nexus might be a good spot to try,
@johnrainy
I would also recommend trying to repost this in the chemistry and pharmacology forum. It is where a lot of the extraction talk goes on.
https://www.shroomery.org/forums/postlist.php/Board/92
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spiritlands



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Re: Psilocin extraction internet recipe [Re: sh4d0ws] 1
#26387758 - 12/17/19 08:14 PM (4 years, 1 month ago) |
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 So I went to find toluene but home Depot didn't have it but they did have this mek substitute. The ingredient is ethyl acetate which is the first recommended substitute for ether. I've never needed ethyl acetate but it's good to see it is otc and there aren't other things in it.
I also bought this 1/2 'T' fitting for $3. This will be our aspirator. You will need a bic ball point pen. Pull the guts out and cut the end off. This should fit pretty snug in thick wall 3/8 tubing. You will also need some half inch tubing.
Edited updated assembly↓

 This is the basic setup. The water pump pushes cold water through the pen tip. The pen should be pushed past the vacuum line but don't let the barrel of the pen obstruct the vacuum line opening. This creates a Venturi high velocity water flows passed the vacuum opening creating low pressure and so it sucks air bubbles out of our vacuum jar and they are washed back into the bucket by siphon effect. This should be able to generate 15-25 psi of vacuum which will boil water at room temp. I will also show you later how to adapt a jar lids to become a vacuum filtration jar which seriously speeds up the process and allows us to use several filters to get our extract free of particulates. You can see the fitting I have for the jar. I drill a hole slightly smaller than the fitting and thread it into the hole. Then I rtv it real well. Try to make it as rigid as possible and have no leaks. I like to use a jar large enough to place shit glasses in it.
The smaller vessel you vap your extract in the easier it is to deal with. It sucks extracting a tiny amount of something and have it coating the whole inside of the jar. So I put solution into a shot glass or two and I add more solution to the glass as it vaps. This concentrates it all into one small vessel which will save you headaches later. Less is more when it comes to solvents.
Edited by spiritlands (12/27/19 04:58 PM)
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