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InvisibleCactilove
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Pure psilocybin extraction TEK * 1
    #16752595 - 08/29/12 05:26 AM (11 years, 7 months ago)

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.

This method permits rapid isolation of psilocin from hallucinogenic mushrooms by co-extraction of both psilocin and psilocybin. Dilute acetic acid is an excellent solvent for this purpose, because both compounds are very soluble in acetic acid11 and very little of other interfering substances are extracted, It is most likely some other compounds are co-extracted but are removed from psilocin in the ether extraction from the aqueous base. Psilocybin is completely dephosphorytated to psilocin by heating the acid extract. After addition of the base, extraction into ether should be performed promptly, because of decomposition of psilocin at a greater pH than 712. The extraction and dephosporylation steps produce reasonably pure psilocin from a small amount of mushroom material. Two grams of mushrooms will often be sufficient to obtain an infrared spectrum of psilocin (Fig. 1). Smaller mushrooms exhibits provide ample psilocin for mass spectral analysis (Fig. 2).
This method has been used in our laboratory for six months and has given excellent results in separating psilocin from methanol-soluble compounds. Other identification techniques such as gas chromatography and microcrystalline tests are possible on psilocin extracted by this method.

Is there any reason I could not replace the Glacial acetic acid with citric acid?

How about ammonium hydroxide? Can I just use baking powder or washing soda? Any other food safe basifying suggestions?

Fuck Ether don't have a supplier and certainly don't want to risk making my own. substitutions? Naptha?

"The ether is dried over sodium sulfate, filtered, and evaporated under nitrogen with no applied heat." What is this nonsense? Does a kitchen Chemist have the ability to do this? Any ways around it?

Heptane Re-X? Will hardware store heptane do? Is it like the same process of RE-Xing DMT crystals?

WIll this come out freebase? If so how do I convert back to a salt?

Any way to easily store the raw crystal as a salt or do I need to keep it in an acidified alcoholic or water solution?

I want a way to get pure psilocybin crystal in a vial that will last for a good amount of time, feasible for a beginner home chemist? At the very least some liquid in a vile concentrated enough to get one good dose off of an ml of liquid. preferably a drop. Psilocybin blotter anyone? What if I wanted to shoot it up? ha ha just kidding:grin:


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Edited by Cactilove (08/29/12 05:31 AM)

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OfflineKief Ledger
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Re: Pure psilocybin extraction TEK [Re: Cactilove]
    #16753309 - 08/29/12 09:51 AM (11 years, 7 months ago)

Ever clear extraction?  Seems to do basically the same thing minus the pretty crystals.  Besides I believe psilo is rapidly oxidized when exposed to the air.

I've been wondering what's the max psilocybinin/alcohol ratio(ie:what's the most psilocybin that will dissolve in the least amount of alcohol).  Could one theoriticelly put say a grams with of actives into a drop of ever clear? That would be so epic!

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Invisiblesailing
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Re: Pure psilocybin extraction TEK [Re: Kief Ledger]
    #16753344 - 08/29/12 09:58 AM (11 years, 7 months ago)

Quote:

Kief Ledger said:
Ever clear extraction?  Seems to do basically the same thing minus the pretty crystals.  Besides I believe psilo is rapidly oxidized when exposed to the air.

I've been wondering what's the max psilocybinin/alcohol ratio(ie:what's the most psilocybin that will dissolve in the least amount of alcohol).  Could one theoriticelly put say a grams with of actives into a drop of ever clear? That would be so epic!



everclear extraction can lead to pretty crystals too, you just have to evap the alcohol. wich alcohol evaporates at low enough temperatures to not ruin the psilocyben.

and i think a could way to test that is to extract a certain amount of shrooms into alcohol, and evaporate the alcohol slowly a little bit at a time until a precipitate forms. this is theoretical of course, im not a chemistry expert.


--------------------
Love is the deep spiritual connection between the self and all things. We are all a part of the same universe.

Crazy cat peekin through a lace bandanna,like a one eyed cheshire, like a diamond eyed jack.

:awecid2:

Edited by sailing (08/29/12 09:59 AM)

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OfflineKief Ledger
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Re: Pure psilocybin extraction TEK [Re: sailing]
    #16753592 - 08/29/12 10:51 AM (11 years, 7 months ago)

I believe the crystals that form in a ever clear extract are oils from the mushrooms,  not psilocybin. They were brown, very greasy, and not solid( like say dmt would be) when i did it.  I didn't evap all the way though.  It would interesting to see if one were to do it with ISO, and evaped all the way if you would actually get active crystals.

I know somebody around here has more shrooms than they know what to do with who wouldn't mind taking one for the team!:smile:

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InvisibleCactilove
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Re: Pure psilocybin extraction TEK [Re: Kief Ledger]
    #16754311 - 08/29/12 01:28 PM (11 years, 7 months ago)

OK so maybe if I evaporated the ethanol slow perfected multiple filtrations then If I got crystals than I could quickly scrape them out throw in a vial and fill it with  co2 or argon gas? What about as far as the acids bases and solvents go guys?


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Orgone Conclusion...Bringing OTD to PS&P since 2007.

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OfflineKief Ledger
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Re: Pure psilocybin extraction TEK [Re: Cactilove]
    #16754384 - 08/29/12 01:43 PM (11 years, 7 months ago)

Just soak in alcohol and evaporate.  If your interested in storage, then do enough so that you can try it when its finished to guage initial potency, and then store for a given amount of time and sample again and compare the results

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InvisibleCactilove
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Re: Pure psilocybin extraction TEK [Re: Kief Ledger]
    #16754494 - 08/29/12 02:06 PM (11 years, 7 months ago)

your sure that will give nice whit crystals I have a feeling it will just give a nasty sludge.


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OfflineKief Ledger
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Re: Pure psilocybin extraction TEK [Re: Cactilove]
    #16754718 - 08/29/12 02:52 PM (11 years, 7 months ago)

Not the least bit sure.

The tek you posted sounds plausible if you have the right chems.  Its just an acid /base extraction
if one wanted to make it a tad safer you could substitute citric acid/pickling lime:shrug:

I can attest to however, that a simple soak in ever clear and evaporated down to a shot works wonders. :aweyeah: My next attempt I shall see just how concentrated I can make it.  If i could get an 8th into 10 ml, that'd be so sweet

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InvisibleCactilove
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Re: Pure psilocybin extraction TEK [Re: Kief Ledger]
    #16754743 - 08/29/12 02:56 PM (11 years, 7 months ago)

Thanks for the acid info. Im looking to getting like a half eighth per drop, now that would be epic.


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OfflineKief Ledger
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Re: Pure psilocybin extraction TEK [Re: Cactilove]
    #16756234 - 08/29/12 07:20 PM (11 years, 7 months ago)

I believe any active amount in a drop would be a cause for celebration

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InvisibleCactilove
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Re: Pure psilocybin extraction TEK [Re: Kief Ledger]
    #16756264 - 08/29/12 07:28 PM (11 years, 7 months ago)

found one Tek that says the best you can do is 1 gram per ml of liquid, still pretty good. I wonder if water can hold more or less.


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Offlinethrdel
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Re: Pure psilocybin extraction TEK [Re: Cactilove]
    #25264985 - 06/13/18 05:44 AM (5 years, 9 months ago)

Quote:

Cactilove said:
A representative sample of 2 to 10g of dried mushrooms ...100 mL of dilute acetic acid in a 250-mL beaker. The pH is readjusted to pH 4 with glacial acetic acid.

Is there any reason I could not replace the Glacial acetic acid with citric acid?

Dilute acetic acid is the regular vinegar . Adding mushrooms to vinegar doesn't increase the pH that much.The article is in scientific terms assuming the reader has access to a proper lab and chemicals. If the pH raises up when adding the mushrooms, adding extra vinegar will drop the pH. Adding glacial acetic acid will require a few drops, adding vinegar requires a few ml. No big deal.

How about ammonium hydroxide? Can I just use baking powder or washing soda? Any other food safe basifying suggestions?

Sodium carbonate and sodium bicarbonate , both introduce sodium and carbonate in your mix. Ammonia evaporates easily from the mix while sodium doesn't, therefore using ammonia is a cleaner way of doing it.

Fuck Ether don't have a supplier and certainly don't want to risk making my own. substitutions? Naptha?

Psilocin is much less polar than psilocybin , hence the higher solubility of psilocybin in water . Water is very polar solvent and psilocin is only slightly soluble in water but soluble in acidic water. Since psilocin isn't very polar , will migrate easier into a non-polar solvent than psilocybin.
Diethyl ether boils at 34.6°C , very easy to get rid of it .So is Chloroform if you have access to it or think it's easier to make. Very close as polarity and boiling point . Acetone is miscible with water so no good, toluene boils at 110°C ,not so easy to get rid of, ethyl acetate may be an option but again , it's boiling point is double the BP of Ether.


"The ether is dried over sodium sulfate, filtered, and evaporated under nitrogen with no applied heat." What is this nonsense? Does a kitchen Chemist have the ability to do this? Any ways around it?

This "nonsense" means that ether will contain water 6g per 100 ml from the extraction . You don't want that water to interfere with crystallization , right ?
How to avoid that ? Drop a little bit of sodium sulfate in , let it absorb the water for a bit and then you filter the ether. Now you have a much drier ether to evaporate. 

You don't need much heat to evaporate ether (BP is 34.6 °C , remember ? ) . Holding the flask or the beaker in your hands is enough heat to quickly evaporate ether.
Don't know why it says " with no applied heat, psilocin can be crystallized from boiling water (100°C) .Maybe is just to avoid oxidation ?
The nitrogen is there to avoid oxidation of the psilocin as much as possible . So it is drying under vacuum .



WIll this come out freebase? If so how do I convert back to a salt?

If your work is very clean you may end up with an oily clear substance . Apparently psilocin doesn't crystallize from ether. You can however re-crystallize from boiling water or boiling methanol , dissolve in acidic water of your choice (citric acid , ascorbic acid , HCl ) , evaporate water and keep the salt. 

Any way to easily store the raw crystal as a salt or do I need to keep it in an acidified alcoholic or water solution?

Psilocin degrades very easy within days or weeks depending on conditions . Some say it is best stored under inert gas at -11°C . If that's not possible , vacuum is the next best thing, still at low temp.

I want a way to get pure psilocybin crystal ...
This tek is for psilocin , not for psilocybin. Psilocybin seems to be  much harder to isolate and crystallize. For more than 60 years people are trying to do that and there's no tek available yet. Everyone knows and can give advise , plenty chemist out there but not one concise method for psilocybin . That should tell something to the amateur chemist looking to get the magic crystals.

...in a vial that will last for a good amount of time, feasible for a beginner home chemist? At the very least some liquid in a vile concentrated enough to get one good dose off of an ml of liquid.
preferably a drop. Psilocybin blotter anyone? What if I wanted to shoot it up? ha ha just kidding:grin:

Since psilocin is slightly soluble in Ethanol and Vitamin C is soluble in Ethanol at about 33g/ L as an anti oxidant , this may be a method of storing it.
As far as the "drop" thing, I don't think it's going to  happen. Since psilocin is not very polar , it needs a lot of water to dissolve or about the same amount of ethanol . The other , much better solvents like acetone , ether and hexane , are not drinkable.
So there you are. There's no easy way to extract and store the magic, at least not yet.
Cheers






Edited by thrdel (06/13/18 06:07 AM)

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