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InvisibleSoopaX
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Registered: 11/13/04
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Write up of anhydrous methanol extraction of psilocybin
    #3764146 - 02/10/05 10:06 PM (11 years, 9 months ago)

This writeup is my own. It is a typed-out, detailed version of ion's tek for this same procedure found at thenook.org. I am not claming this as my own, mearly typing out the procedure that I would recommend and seeing if it sounds like it is copacetic with ion's or anything that you are familiar with.

Extraction of psychoactive indoles from psilocybe fruits

Scope: Detail the methodology for extracting the maximum amount of psychoactive alkaloids from cultivated p. cubensis mushrooms. The equipment necessary, sources and all appropriate steps and preparations will be discussed in enough detail that they may be easily reproduced.

Purpose: The goal of this experiment is to end up with an extremely pure, crystalline product containing only the psychoactive alkaloids found in the fruit bodies. The expected alkaloids to be extracted are psilocybin, psilocin and baeocystin. The process will start with the fruit bodies of the fungus and will finish with a crystal product.

Equipment:
Buchner filter Vacuum pump
1000mL Erlenmeyer flask 250mL Erlenmeyer flask
1000mL filtering flask 250mL filtering flask
Rubber stoppers for Erlenmeyer?s 1000mL lab beaker


Materials:
Dried p. cubensis mushrooms Methyl Alcohol, anhydrous
Calcium chloride (CaCl)

Procedure:

I. The first step is to totally dry as many of the materials as we can. The mushroom fruits are dried over a fan for 24 hours and then placed in a desiccant chamber using Damp-Rid. After they were dry to the touch they were ground up into a powder and placed on a Petri dish and subjected to another 24 hours in the desiccant chamber. They were then placed in the freezer.

The methanol that you have should be totally anhydrous but it will absorb water from the atmosphere quickly. If it is chilled thoroughly it will absorb at a slower rate and remain anhydrous longer. Fill a 1000ml Erlenmeyer with methanol and shake it around some. Pour the methanol out and do NOT reuse for this procedure. This will empty any humidity and get rid of any gasses present in the flask.. Now pour about 650mL of methanol into the Erlenmeyer, place the rubber stopper in it, cover with some aluminum foil and place it in the freezer. We will need another flask of methanol for wiping up behind us and getting all of the mushroom powder. Do this procedure with a small 250mL Erlenmeyer as well, putting about 200mL of methanol in it. A 10? glass stirring rod should be wrapped in paper towels and placed in the freezer as well. Keep the methanol, the mushrooms and the stirring rod in the freezer for at least 2-3 hours so that they chill completely.

II. Now that we have our chilled solvents and solute it?s time to extract! Dr. Shulgin states that some analysis of mushroom alkaloid content might not be totally accurate in the category of psilocin. He feels that a long soak is necessary for the methanol to get into the cell structure and absorb all of the psilocin. That?s how we?ll do it then!

A desiccated glove box is used for this procedure. This is accomplished by placing an open tray of Damp-Rid in a regular, sealed glove box for about two hours. The methanol flasks, mushroom dish and stirring rod are all removed from the freezer and moved into the glove box. A glass funnel is placed in the Erlenmeyer and the mushroom powder is poured in from the Pedri dish. The 250mL flask of methanol can be poured in the dish and swirled around a few times to get any mushroom particles out and poured in with the larger flask of methanol. Re-cork the large flask as soon as the powder and liquids are poured in.

Invert the jar a few times and slightly uncork it to release some pressure. Do this 10-15 times so that the methanol totally saturates the mushroom powder. Now it?s time to let the solvent dissolve things. Place this flask, corked well, in your incubator (80-85?F) for 2-3 days, inverting and releasing pressure every day.

III. By now the methanol hopefully has dissolved all of the psychoactive chemicals in our mixture. We?ll cool it in the refrigerator a little bit so that all of the mushroom powder particles will drop out of suspension in the methanol and we end up with less foreign matter in our finished product. Then we?ll filter the methanol to remove all of the mushroom powder and be left with methanol and the dissolved psychoactive substances.

Put the Erlenmeyer in the refrigerator for about two hours. I?m still not sure if this step is really required but it doesn?t hurt anything or cost anything, so why not do it until we have conclusive proof that it?s a waste of time? All of the fungal mass should drop out of the methanol and be on the bottom.

Pour this through a filter paper and vacuum filter into the 1000mL filtering flask. Now it?s just a matter of allowing the methanol to evaporate. Pour the methanol into a Pyrex dish and place on a heating pad in front of a fan. Methanol will vaporize quite quickly and leave you with a powdery substance after it?s gone. As it?s possible that some water may have gotten in the methanol at some point it?s a good idea to desiccate your powder. Place the Pyrex dish in your desiccant chamber overnight so they are totally dry. You can stop here or continue to step IV for crystallization

IV. To obtain the most pure product we must crystallize the alkaloids. I?m going to type this all up in one step since we are familiar with the techniques as previously described.

We?ll be using VM&P Naphtha as our crystallizing solvent. We want it as cold as possible so that the crystals that we are looking for precipitate out of the solution. You can just place your metal can of VM&P in the freezer for a few hours for preparation. When the naphtha is thoroughly chilled remove the can from the freezer. Pour about 20mL of naphtha into the Pyrex dish. You want to use just enough to absorb all of the crystals. Put the cold naphtha and psilocybin mixture into an 250mL Erlenmeyer and place in the refrigerator for 15-20 hours and then into the freezer overnight. All of the crystals that precipitate from the naphtha are the crystalline form of the compounds that we sought after. Set up your Buchner filter again and vacuum filter those crystals. Rinse the Erlenmeyer out with cold naphtha and pour into the filter. Leave the vacuum on until the crystals are totally dry. After this step, if you desire, you can place a Petri dish of these crystals back into your desiccant chamber before you store them.


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


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OfflineRandolph_Carter
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Re: Write up of anhydrous methanol extraction of psilocybin [Re: SoopaX]
    #3770277 - 02/12/05 09:36 AM (11 years, 9 months ago)

You may want to bake some epsom salts to dryness and add those to the methanol, to hunt down that inevitable 5% of water.....(place in oven, bake 300f for a few hours)
They're pretty inactive too(and are insoluble in alcohols), so can be left in during the entire extraction procedure. A goodly amount of those would go a long way towards keeping you anhydrous.

There remains the possibility of some cellulose dissolving and making it thru to the crystallization, but it shouldn't be a large amount.

The evaporation of methanol will STINK.

But it'll work the way you've described it.


--------------------
"..all those molecules thrashing their kinky little tails, hot for destiny and the street."  Gibson


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Offlinebobmarley4prez
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Re: Write up of anhydrous methanol extraction of psilocybin [Re: Randolph_Carter]
    #3778088 - 02/14/05 12:03 PM (11 years, 9 months ago)

so would dryed epsom salt work to "dry" methanol?


--------------------
Anything above this line is a lie. i do not cultivate psychadelic mushrooms nore do I intend to.

One day I encountered a bufo toad. Since that day I have been instilled with the power of the devil.


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OfflineRandolph_Carter
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Re: Write up of anhydrous methanol extraction of psilocybin [Re: bobmarley4prez]
    #3781156 - 02/15/05 12:06 AM (11 years, 9 months ago)

Yes, but you've gotta bake the shtuff first.
And then you've gotta keep the methanol out of contact with the atmosphere, otherwise the work is lost as it will pick up any availible moisture to get back to azeotropic form.


--------------------
"..all those molecules thrashing their kinky little tails, hot for destiny and the street."  Gibson


Nuke baby seals for Jesus!

(This has been a +1 production.)


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OfflineRugbyhooker
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Re: Write up of anhydrous methanol extraction of psilocybin [Re: Randolph_Carter]
    #3781913 - 02/15/05 03:10 AM (11 years, 9 months ago)

I find just eating them gets plenty of alkaloids out of the fruitbodies.  :tongue:  Now finding a way to extract the alkaloids out of spent casings would be a truly worthwhile endeavor.


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Slowcoaster


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Offlinepyronicx
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Re: Write up of anhydrous methanol extraction of psilocybin [Re: Rugbyhooker]
    #3782046 - 02/15/05 04:18 AM (11 years, 9 months ago)

Won't the psilocybin and psilocin oxidize very quickly and making the potency of the crystals drop rapid ?
Would be better if you could work in a inert gas but i think that is for ppl with access to a lab =]


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OfflineRandolph_Carter
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Re: Write up of anhydrous methanol extraction of psilocybin [Re: Rugbyhooker]
    #3782339 - 02/15/05 08:04 AM (11 years, 9 months ago)

The outlined procedure would work for casings as well.

Pyro: CO2 is relatively inert, and easily had.


--------------------
"..all those molecules thrashing their kinky little tails, hot for destiny and the street."  Gibson


Nuke baby seals for Jesus!

(This has been a +1 production.)


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Offlinepyronicx
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Re: Write up of anhydrous methanol extraction of psilocybin [Re: Randolph_Carter]
    #3806072 - 02/20/05 09:31 AM (11 years, 9 months ago)

Quote:

Randolph Carter said:
The outlined procedure would work for casings as well.

Pyro: CO2 is relatively inert, and easily had.




i know i store my shroom powder in co2 from the reaction of soda with acetetic acid.


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Offlinetofey
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Re: Write up of anhydrous methanol extraction of psilocybin [Re: pyronicx]
    #3806197 - 02/20/05 11:23 AM (11 years, 9 months ago)

If anhydrous methanol is difficult to get without a permit, what about with adding calcium chloride directly to 95% alcohol (Everclear) to dry it? I.e., how much CaCl per volume of 95% alcohol would be needed and how long should it stay in to "dry" the alcohol? Can this be left in for extraction process?


--------------------
"Simplify, simplify, simplify." -- Henry David Thoreau


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