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freeze precip of psilocin Options
 
kaos.underwave
#21 Posted : 11/10/2009 9:55:04 PM

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brilliant... don't you wonder what vaping spice and psilocin together would be like... something new
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69ron
#22 Posted : 11/15/2009 9:19:41 PM

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soulman wrote:
69ron wrote:
soulman wrote:
69ron wrote:


Dried mushrooms that were steam treated after drying and then dried again seemed to maintain their potency far longer.

SWIM really hopes his frozen mushroom are ok. They were dried before freezing them. They are MANY YEARS OLD, I think they are 15 years old? I’m not sure.



What does steam treating dried mushroom do that makes them keep their potency?...Could you do this by placing them in a corrinder over a steamin pan?

Also, why you keepin them in the freezer for that long man. You really find them that hard to come by?


Yeah, just steam cook the dried mushroom like you’d cook any other vegetable. Cook for about 5 minute or until the mushrooms lose all their blue color. Break one open to be sure it’s lost it’s color all the way through and it’s done. Steaming inactivates enzymes present in the mushrooms that oxidize psilocin to an inactive blue substance. It’s also believed by some that it reverses the oxidation, but there is no proof of that. Some people think it hydrolyzes psilocybin to psilocin, again, no proof of that either. If the steaming converted the psilocybin to psilocin, it seems that the steamed mushrooms would not keep well, but they do, so I don't know if that happens.


At what point does this have to be done?
As soon as they are dry?...or does it matter if they have been dried for awhile?
Im all for trying this, but still dont really get it. Surely, if the mushrooms are already dry the enzymes arent gonna be active anyway. I might be wrong about that, but i wouldnt have though enzymes can function in arid conditions?!!
Can you explain that bit to me please?


It can be done at any point. They should be dried first though.

The enzymes that oxidize psilocin to a blue compound are still present in the untreated dried mushrooms. You can easily test that out by making a smoothie out of the dried untreated mushrooms and letting it sit overnight. The next day the liquid will be colored dark blue, and the potency will have reduced dramatically. But if you use steam treated dried mushrooms, the smoothie will not turn blue, and will be highly active the following day.

Why not try it with just one mushroom and see for yourself?

As far as how this works, I’m not really sure. I don’t know the name of the enzyme that turns psilocin into an inactive blue compound, and I don’t know the name of the blue compound either, so it’s very hard to research it.
You may remember me as 69Ron. I was suspended years ago for selling bunk products under false pretenses. I try to sneak back from time to time under different names, but unfortunately, the moderators of the DMT-Nexus are infinitely smarter than I am.

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Oncewas
#23 Posted : 11/15/2009 9:38:13 PM
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I was told only psilocin was vaporizable and was considered to be like dmt, but longer in duration and more intense.

I'd hate to be the guy who messed up trying this several times however. Hence why I have never tried it.
 
benzyme
#24 Posted : 11/15/2009 9:39:00 PM

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69ron wrote:

The enzymes that oxidize psilocin to a blue compound are still present in the untreated dried mushrooms.


this makes sense
as long as the enzymes aren't denatured by high heat in the dried material, they remain inactive until activated in an aqueous environment.
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Phlux-
#25 Posted : 1/14/2010 5:24:49 AM

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doesnt the greenish color show oxidization ?

me! did a thread on getting xtal psilocin in 4 hours on the nook a while ago
here is the link
http://www.thenook.org/f...mp;hl=mescaline&st=0
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imPsimon
#26 Posted : 1/14/2010 2:38:54 PM

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Phlux- wrote:
doesnt the greenish color show oxidization ?

me! did a thread on getting xtal psilocin in 4 hours on the nook a while ago
here is the link
http://www.thenook.org/f...mp;hl=mescaline&st=0


I cant see the nook page, think one must be a member.

Cant you post it in the mushroom subforum here at the nexus?

=)
 
Phlux-
#27 Posted : 1/14/2010 2:58:38 PM

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its 5 pages, im lazy, its quicker to register.
antrocles wrote:
...purity of intent....purity of execution....purity of experience...

...unlike the "blind leading the blind". we are more akin to a group of blind-from-birth people who have all simultaneously been given the gift of sight but have no words or mental processing capabilites to work with this new "gift".

IT IS ONLY TO THE EXTENT THAT WE ARE WILLING TO EXPOSE OURSELVES OVER AND OVER AGAIN TO ANNIHILATION THAT WE DISCOVER THAT PART OF OURSELVES THAT IS INDESTRUCTIBLE.


Quote:
‹Jorkest› the wall is impenetrable as far as i can tell


Quote:
‹xtechre› cheese is great


He who packs ur capsules - controls your destiny.

 
narmz
#28 Posted : 1/17/2010 7:26:18 PM

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benzyme wrote:
it's an a/b to first convert psilocybin to psilocin, then to free base.


Why do you freebase?
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Otiliya
#29 Posted : 1/20/2010 9:48:21 PM

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pasted from the nook:

The following method described shows an easy method to isolate pure psilocin from fungus in less than 4 hours. If a more pure product is wanted, the fairly pure psilocin can be recrystallized to produce large pure crystals.

20 grams of dried fungus is powdered in a coffee grinder to a fine powder. This is added to a glass container (~500 ml) along with 200 ml of distilled water and 40 ml distilled white vinegar (5% acidity). ~200 mg of vitamin C was also added to keep the psilocin from decomposing. This mixture was allowed to stir at room temperature for 1 hour and then the container was placed in a bath of boiling water to heat the mixture to 70 degrees C. After the mixture reached this temperature, it is filtered through multiple coffee filters (3-4 is good) and the filtered (be sure to squeeze out all the juice!) liquid is set into a cold water bath to cool it down. The extracted fungus is recovered and put into another container along with 150 ml water and 20 ml vinegar. This is again heated to 70 degrees C and then filtered as before. The filtrate is again cooled down and then added to the 1st extraction. The combined filtrates should give somewhere around 300 ml of liquid. Add about 30 ml of chloroform (xylene should also work, as psilocin is solubile in this as well) and begin stirring gently (you don't want emulsions, do you?). While stirring, SLOWLY add NaOH solution (~10 % NaOH is fine). I would suggest a drop by drop addition, as the pH can raise raphidly after a certain point. Target pH is 8, just try not to go over pH 9, as the alkaloids can decompose pretty fast at high pH. After the pH is at 8-9, continue to stir gently for about 20 minutes (electric stirrers are nice) and the psilocin will migrate into the chloroform (or xylene) layer. This is poured into a separatory funnel (or something similar) and the bottom chloroform layer is removed and set aside. The water layer is again stirred and 15 ml of chloroform is added for a second extraction. After 20 minutes of stirring, this is again separated in a separatory funnel and the chloroform recovered. These two chloroform extracts are combined and put into a small beaker. To this beaker, anhydrous MgSO4 is added (just oven dry epson salts in an oven at 450 degrees F for about an hour) to absorb any water. Usually only a gram or so is needed. Stir the chloroform with the MgSO4 for a minute or so and then filter through a "good quality" filter paper so you catch all the fine particles. The resulting chloroform layer will have a light yellow color. Now you have two choices:

You can evap the chloroform quickly to yield a fairly pure psilocin powder, or let it evaporate slowly to get larger and more pure crystals. Recrystallization can be carried out with methanol or a 3:1 heptane:chloroform. The recrystallized material is very pure and 20 mg is equivelent to 4-5 grams of mushrooms. Average yield for this method is about 60 mg of pure crystals (after recrystallization). The crystals do decompose at room temperature over time. The yellow crystals turn green in about a week or so if left out. To preserve the psilocin, put ~50 mg of psilocin in a small container and add ~50 mg ascorbic acid and 20 ml water. The psilocin will dissolve, but it does so slowly. You now have a solution with 2.5 mg psilocin per ml. This can be stored for many months in the refrigerator (possibly longer). An interesting note is that this "psilocin water" can be evaporated to give white needle crystals which don't seem to degrade at room temperature. Perhaps this is the way to stabilization!
pic 1
pic 2
pic 3
Yes, it is 60 mg, but this is after recrystallization. The "crude" material was 90 mg. I would estimate the extraction to be about 70% efficient, as it provides 3 ~5 gram trips. Also remember that psilocin is about 30% more potent than psilocybin by weight. It is somewhat hard to tell the actual efficiency, as it is all objective for now.

Triptamine
 
Otiliya
#30 Posted : 1/20/2010 10:34:22 PM

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Here's another one from the nook by ion:

Sure I can help! I'm glad you asked smile.gif

Ethanol is NOT the best solvent in the world to use for 2 reasons:
a. it contains water (making it a bitch to evap and work without heat)
b. ethanol does not extract psilocybin very well... (water does, better at least, though it still isn't so great. acidic water works well, but it's still water)

The best advice I can give you is this: Find some pure methanol. Read my journal threads on kitchen chemistry and sources.

You will need the vacuum filter for a different purpose (one which very few people know wink.gif )...

Grind dry mushies to a powder. Seal the powder in a jar (make sure the level of the powder is AT MOST only half the volume of the jar) and freeze it until you are ready to use it. Refrigerate some methanol. Take the jar of powder out of the freezer... QUICKLY open the methanol jar, then the powder jar, and swiftly add the methanol to the powder about an inch (small jar) or half inch (large jar) above the level of the powder, and QUICKLY seal the mixture jar.
*I say "quickly" because cold jars will gather water condensate from the surrounding air... this will mix with alcohol... this will really suck later. It is best to do all of these procedures in a dessicated glove box (just a bowl of Ca chloride set in the glove box for an hour prior to work).*

Swirl this slurry (methanol+powder) around for about half an hour, relieving pressure every couple minutes (warming alcohol will expand gaseously, so pressure relief is necessary for safety, though I doubt the jar will actually pop or anything...). Let the slurry settle and pour the alcohol through a funnel, filtered by either:
a. vacuum filtration through filter paper (this may clog, though)
b. a layer of dense fabric (high knit sheet or shirt) with a coffee filter on top. This will be squeezed to remove last liquids.

The leftover crud (filter cake) can be extracted by repeating the methanol extraction outlined, or it can be thrown out. You will probably want to re-extract the first few times, until you get the hang of doing this perfectly.

Evaporate the methanol by blowing over the jar with a fan... this, too should be done with dessicated, de-oxygenated air, but the apparatus is too complex to build for description here... it may be in my kitchen chemistry chat posts ??

As you evaporate, you MAY see crystals... maybe not. Either way, continue evaporating to dryness.

This residue may be eaten in doses of about 3 times that you would take of pure psilocin (30mg residue = 10mg psilocin)... this depends on the strength of the shroom (that's why crystal would be better, because you would KNOW how much goodie you are eating). If you have crystals, just measure them directly as weight of psilocin.

BTW, this is a mixture of psilocin and pilocybin... I only say psilocin for the sake of brevity, in that psilocin is the more potent molecule by weight. Most of the mix will be psilocybin, but it is better to err to the lower end of dose.

Here's the big trick to decent purification of these compounds:
Dissolve the residue and/or impure crystals in room temp. petroleum ether (in this case, you can use zippo fluid). You may notice that crystals don't dissolve well, though they might (because of impurities). Only add enough pet. ether to get the stuff suspended/dissolved as you stir... if crystals won't dissolve, DON'T add more pet. ether. Crystals not dissolving is GOOD!

Close the container you are doing this in and put it in the fridge. When it gets to fridge temp, put it in the freezer. (Slow cooling forms bigger crystals ). Leave in freezer until you see no more crystal growth (overnight, usually).

Stir up the mix (still freezing cold) with a cold stirring rod, suspending the crystals in the liquid. Swiftly pour this into the vacuum filter apparatus and flip it on. Rinse the container with a bit of more freezing cold pet ether, and dump this into the filter. You want to get every last crystal, right?

Leave the vacuum on until the crystals are dried by the air (again, preferably dessicated and de-oxygenated). This is a relatively pure crystalline mix of psilocin and psilocybin.

Depending on experience and perfectionism, the yeild from a single methanol extraction (no re-extraction of the mushy filter cake) of this caliber is approximately 95%. Most losses occur from oxidation, over use of solvents, bad temperature control, and transfers (leftover drops in containers).

To store this pure product, get some pure ascorbic acid (vitamin C) crystals. Dissolve some of the vit. C in twice it's volume of 190pf ethanol. Now, dissolve your cin/cybin crystals in this acidic ethanol.

Put this mixture in a dark container (something opaque) in the freezer.

That's it!

-ion




I wonder if a FASA/FASI can be thought of using limonene for psilocin salts.
 
benzyme
#31 Posted : 1/21/2010 12:14:55 AM

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narmz wrote:
benzyme wrote:
it's an a/b to first convert psilocybin to psilocin, then to free base.


Why do you freebase?


because that's usually what you do after acidifying an alkaloid...convert it to a free base. what you do after that is up to you.

Otilya, those nook pieces leave out some important points..
for starters, neither of those methods gives pure psilocin/psilocybin; both pull proteins (enzymes) as well, which is why crystals will turn greenish. column chrom and/or AC will definitely clean it up via size exclusion, enzymes are pretty bulky macromolecules. the other option is sublimation under reduced pressure
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VisualDistortion
#32 Posted : 1/21/2010 4:41:00 AM

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Is tartic acid soluble in DCM? Could psilocin tartrate be crashed out by adding a saturated solution of DCM/tartaric acid?
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VisualDistortion
#33 Posted : 2/16/2010 3:38:17 AM

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VisualDistortion wrote:
Is tartic acid soluble in DCM? Could psilocin tartrate be precipitated out by adding a saturated solution of DCM/tartaric acid?


Can any of our chemist here answer this question. For the life of me I cannot find any DCM in my town. but I do not have any alks to attempt to precipitate anyways.
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benzyme
#34 Posted : 2/16/2010 3:50:47 AM

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hmm..

if it were possible to get a bitartrate salt of psilocin, I'd say yes..it may be possible to get it to crash out in cold DCM, but it's not possible.
as psilocin tartrate, it would probably go into solution. worth experimenting with, though, since dcm evaps easily
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VisualDistortion
#35 Posted : 2/16/2010 4:48:19 AM

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benzyme wrote:
hmm..

if it were possible to get a bitartrate salt of psilocin, I'd say yes..it may be possible to get it to crash out in cold DCM, but it's not possible.
as psilocin tartrate, it would probably go into solution. worth experimenting with, though, since dcm evaps easily


Really? The bitartrate salt of psilocin would probably go into solution in DCM? I'd expect it to crash out, but maybe DCM is to polar for that. My chemistry knowledge is very rudimentary so excuse my learning curve.
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benzyme
#36 Posted : 2/16/2010 4:58:48 AM

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no
sorry for the confusion..i meant if it were possible to bind two tartrate ions (it's not), then you could theoretically crash it out in dcm.

ascorbate is another good candidate
"Nothing is true, everything is permitted." ~ hassan i sabbah
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VisualDistortion
#37 Posted : 2/16/2010 1:23:48 PM

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Why would it need to be bitartrate? I thought ascorbic acid and tartic acid where very similar anyways.
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PlainCoil
#38 Posted : 2/19/2010 10:17:56 PM

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Idea:

Steam treated shrooms extracted with warm vinegar water. Vinegar water is filtered several times and given time for particulates to settle.

Clarified extraction is basified with sodium carbonate.

Will the freebase crystals fall out? If not, the whole lot could be evaporated and the resulting material re extracted with warm 99% IPA. This should leave behind the base and pick up the alkaloids only - if the alks are reasonably soluble in IPA.

When dried, this crude extract should contain a good deal of freebase psilocin, correct?

This could be piled in between some herbs in a vaporizer whip could it not?
 
benzyme
#39 Posted : 2/19/2010 10:51:10 PM

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nice ideas
psilocin is both photosensitive and air-sensitive, the latter being more of an issue.
anything that oxidizes what little yield is there, will render it inactive.

a dirty bird is working on an inert-environment tek for several purposes.
nitrogen is readily available from welding supply stores
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benzyme
#40 Posted : 2/19/2010 10:54:06 PM

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VisualDistortion wrote:
Why would it need to be bitartrate? I thought ascorbic acid and tartic acid where very similar anyways.


qualitatively, they are

the problem is, dcm can interact to some degree with polar molecules, despite not having any proton-donors or acceptors.
it's odd like that
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