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how to further refine 96% ethanol extracted psilocybin crystals?

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lorax

Rising Star
hey!

SWIM just did an ethanol extraction and has a big heap of crystals of varying purity. SWIM would love to further refine those crystals to nearly pure psilocybin.

also SWIM would find it very interesting to know if there is a procedure for converting psilocybin to psilocin? SWIM would like to try pure psilocin. he knows it doesn't store well -he would convert it right before use.

thanks in advance!
 
well, you don't need to refine them futher if you want to convert it to psilocin. you'd just need to do an a/b extraction, using acetic acid (vinegar would work), and ammonia; extract with DCM, recrystallize with heptane.

suggested pHs: 3 and 9 (work quickly during basification, psilocin gets degraded at high pH).

as you can see, the extraction isn't too different from dmt extraction, but don't let the pH get too high for the aforementioned reason.

psilocin is more potent by weight, and some people report a "cleaner trip".

to make these compounds more stable, use aqueous ascorbic acid (a natural antioxidant) to convert the final product into an ascorbate salt; evap off the water (desiccator would work best)
 
what's the need to make it anymore potent?

Seems like you'd only have to take a bit...

Personally I don't see any point in extracting mushrooms, the little dudes are potent enough!
 
first of all SWIM likes dosing with pure substances because the approach to this is more scientific and one knows exactly what to expect. another thing is that there are more forms of application with pure substance. you can for example vaporize it which results in a total different experience. then another thing is the storage.. mushrooms tend to loose potency over time. and rather than having a few kilos lying around SWIM rather has a few little bottles filled with white powder, covered in alcohol to avoid oxidation. plus the effect is somewhat different. you don't get stomach problems.. fungal tissue is very hard to digest. which can result in uneasy stomach feelings, alot of farting, burping and if you're unlucky even diharrea. higher doses are experienced with much more ease and less body load.
 
I was going to comment futher, but this really isn't the place. I know it will spark a large debate.

Would you like me to start another thread to explain my philosophy on the subject?
 
you can, if you'd like. though it really has nothing to do with the pharmacology of it, the potency factor isn't really the issue; just a footnote.
many people don't like the taste of mushrooms, they can't stomach it; and it takes grams of dried material to get an effect.
an extraction bypasses all that cellular material to isolate the goodies, it's a just convenient way of reducing the material to its active components. 15-20mg extract vs. 3g raw material... that's like one size 5 capsule vs. six size 00 caps.

and its a good way to brush up on extraction techniques.
 
i would love to smoke psilocin/psilocyban
thats what i see this useful for, and academic/medical research

im really impressed youve taken the time and effort to refine the most potent of natural hallucinagens to an even more pure form

kudos

ps, pm
 
cheech said:
hey!

SWIM just did an ethanol extraction and has a big heap of crystals of varying purity. SWIM would love to further refine those crystals to nearly pure psilocybin.

also SWIM would find it very interesting to know if there is a procedure for converting psilocybin to psilocin? SWIM would like to try pure psilocin. he knows it doesn't store well -he would convert it right before use.

thanks in advance!

Cheech,

Could you give us your method of extraction. I've done the ethanol extraction before, but never get anything crystaline, mainly a gooy, smelly extract. I'd love to know what you do and how you do it!

I'm quite anxious to try the A/B on mushrooms...I had read it was impossible because psilocybin is a zwitteron (or something like that) and doesn't form salts. Granted my chemistry is worse than my spelling so I really don't know what I am talking about and my source (wiki) is about as unreliable as Windows Vista.
 
haha, yeah vista sucks.


merck entry- psilocybin

Properties: Crystals from boiling water, mp 220-228°;
from boiling methanol, mp 185-195°. uv max
(methanol): 220, 267, 290 nm (log 4.6, 3.8, 3.6). pH
5.2 in 50% aq ethanol. Sol in 20 parts boiling water,
120 parts boiling methanol; difficultly sol in ethanol.
Practically insol in chloroform, benzene.

Melting point: mp 220-228°; mp 185-195°

Psilocin

Properties: Plates from methanol, mp 173-176°.
Amphoteric substance. Unstable in soln, esp. akaline
soln. Very slightly sol in water. uv max: 222, 260,
267, 283, 293 nm (log 4.6, 3.7, 3.8, 3.7, 3.6).

Melting point: mp 173-176°

also consider, the alcohol extraction will mainly pull psilocybin, as psilocin takes patience extracting (it's embedded in in cellular tissue). an a/b extraction converts the psilocybin to psilocin, acid catalyzed dephosphorylation under gentle heat. protonation of the phosphoryloxy moeity (at a pH ~3) removes the phosphate and replaces it with a hydrogen.

an a/b extraction will give you a dark green goo, which needs be recrystallized (dissolved in hot heptane, then slow evap). a wash in cold ethyl acetate and vacuum filtration prior to re-xtallization may help clean it up
 
Sweet, let me know.

This might be a great way to get rid of the large amount of dried fungus taking up space in my freezer. 4oz turned into 2-3 vials!! YAY!
 
hehe

swim has an actual spice carousel someone gave him, he'd like to fill them with magic spices.

was just thinking, the fumarate salt tek posted by 69ron may work in converting the psilocin free base into crystalline salts. or perhaps a variation of it using ascorbic acid, since it is a good antioxidant. this is another experiment swim will have to look into.
 
to acolon_5: i usually got a gooey residue which could be dried to a hard resin after waiting a few days. i recently found out that the procedure i was using (standard 96,6% ethanol extraction) was the way to go but that my filtering was poor. its all about the filtering. the problem is if you crush the mushrooms into powder, the powder will be so fine that it will easily go through most filters. your alcohol should be mostly clear with a slight greyish tint to it. be sure to always filter when the solution is still hot. otherwise you will loose alkaloids in the filtering process.

also if you squeeze the filter to get the rest of the liquid out, dont add the squeezed stuff to your finely filtered stuff. it will hold alotta gunk you dont want. squeezing seems to push the gunk through the filter. save the squeezed stuff in a different container and do some extra filtering on it or just let it dry out seperately for a crude unrefined extract which can still be used otherwise. i usually redissolve the gunky stuff in 70% ethanol to make a kind of tincture of it. this is quite nice to have on the road when you got no measuring equipment. you'll have to test the potency of that stuff for yourself tho.

it seems to be somewhere between 30 & 50% alks.

it is also very good to often redissolve the stuff in more 96% ethanol and let it sit around for 2 days undisturbed. there will be fine sediments which will settle to the bottom. i usually add those sediments to my gooey crude extract so i will not loose anything. in the process i also save up all the water used to clean out the jars and pour it all into one glass. this will hold a nice trip when you're finished processing 50-100g of cyanescens :)

if using shrooms high in psilocin content i usually do my standard ethanol extractions (i usually extract about 3-4 times) then i do another extraction with methanol since psilocin seems to be more soulable in it. this will not result in much. maybe 5-10 hits from 50g of cyans.

this is how i do it. i have found that one can improve many things.

for filtration i use a combination of spread out cigarette filters, coffee filters and a aquarium pump filter.

patience is the main factor for the whole process. and it costs alotta money because of all the ethanol you need to use. i would never sell my extract since it is of much more value then the mushrooms themselves.

i usually need 2 liters ethanol for 75g of mushrooms. its fuckin expensive.. here it costs like 35 euro per liter.

i had a very enlightening journey yesterday evening from what i thought i had extracted from one gram cyans. man this was potent. i actually had thought of having done too much at one point.

its also fun to clean out the residue from the glassware with some weed. i save up this weed for smoking it on shrooms. it enhances the trip alot!
 
Thanks! I had a sneaking suspicion that mine was just not filtered enough. Also I have noted that IPA does a poor job at extractions compared to ethanol.
 
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