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Recrystallizing Psilocybin

Migrated topic.
benzyme said:
honestly, I'd suggest getting some SPE columns from e.bay, and practice doing A/B through those; i.e. grind your material, acidify it and let sit in a hot water bath at 50C for half an hour, filter, pour solution through the SPE column to saturate it, and pour dilute ammonia (pH 9-10) through it. extract with ethyl acetate or dcm, salt with alcoholic tartaric acid.

to regenerate the columns, pour saturated saline solution through them.
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What size column do you recommend benzyme, will pet ether work instead of dcm, and acetic acid
 
benzyme said:
pet ether will work for recrystallization (don't pour that or dcm through a plastic column), dcm is for extraction from the basic phase.

acetic acid is used to protonate, not extract.
the size of column will depend on the amount of material being extracted. 10mL columns would suffice.
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Cheers benzyme, I'm still learning and thinking as if I was extracting dmt that's why I asked about Pet ether and acetic acid because you mentioned a/b
 
the acetic acid can be used to dephosphorylate psilocybin to cationic psilocin (positively charged psilocin), especially when subjected to gentle heating, which is why I suggested the hot water bath. In that charge state, the alkaloid is fairly stable.
It's when you basify it that you want to extract quickly, using dcm, ethyl acetate, or ethyl ether. from that, you may add an acidic alcohol solution. this is A/B/A.

now that I think about it, dcm will mix with the alcohol...you'd have to evaporate the solution.
ethyl ether or ethyl acetate should form layers. collect the bottom layer and freeze precipitate, or evaporate.

this will yield an alkaloid salt. if anyone is successful crystallizing freeform psilocybin, let me know. It's no simple undertaking.
Crystals of the Gods is a bit misleading. it's not as easy as crashing out in ethanol, some partitioning is in order.

this one can be scaled up https://www.anoniem.org/?https://www.erowid.org/archive/rhodium/chemistry/psilocin.extraction.html
and it cannot be stressed enough, to extract from the basic phase asap, don't let it sit.
 
Code: 
pet ether will work for recrystallization

Wow that's news to me. I've thought dcm & chloroform were already stretching the envelope.

Benzyme, what are your thought on denaturation? Would Psilocybin be able to bind to single amino acids? And more importantly, would already complexified Psilocybin be able to be denatured?

I've used hot dry ethanol(1% MEK) to extract over the period of many weeks. 3-4 pulls iirc.
I've attached two pictures. The last go I had three different fractions. The gunk one was the first one. Hygroscopic, active but barely useable except orally. The majority of 'mushroom perfume' was in that fraction.

The fraction following that was the one on the other picture. Please note that most of the discoloration is from being stored at open air for many months (in a room that was smoked in). Very active, but smokeability a bit is hindered by imho the polysaccharides getting reduced to carbon & forming a heatshield around the material, as ash tends to do.

I had another fraction, which is unfortunately gone already, which was the most active one.
It had no chalky or casein-like chunky proteinlook to it. Pure white, there were at least some polysaccharides still left in there. But smoking worked okay, still I didn't manage to reach breakthrough. I didn't try very hard though, I used most of that for micro & sleep doses.

Considering the pH sensitivity, using dry sulfuric acid to reduce the sugars and reextract would be out of the question, would it benzyme?

The smoked effects were most interesting. The bodyhigh was very similar to mushrooms. But the visual effects were something else entirely. Much closer to DMT than mushrooms, but still very different. Hard to describe, but the visuals were not in the usual symmetric & proportionally even grid pattern like mushrooms, but completely erratic. Much more chaotic, but still nice. Slow buildup after smoking, very constant effects with no discernible peak. Last everywhere from 20 to up to 30 minutes.

EDIT: Attaching pictures does not work for some reason. I'll try again in the next post, I guess?
 
benzyme said:
the acetic acid can be used to dephosphorylate psilocybin to cationic psilocin (positively charged psilocin), especially when subjected to gentle heating, which is why I suggested the hot water bath. In that charge state, the alkaloid is fairly stable.
It's when you basify it that you want to extract quickly, using dcm, ethyl acetate, or ethyl ether. from that, you may add an acidic alcohol solution. this is A/B/A.

now that I think about it, dcm will mix with the alcohol...you'd have to evaporate the solution.
ethyl ether or ethyl acetate should form layers. collect the bottom layer and freeze precipitate, or evaporate.

this will yield an alkaloid salt. if anyone is successful crystallizing freeform psilocybin, let me know. It's no simple undertaking.
Crystals of the Gods is a bit misleading. it's not as easy as crashing out in ethanol, some partitioning is in order.

this one can be scaled up https://www.anoniem.org/?https://www.erowid.org/archive/rhodium/chemistry/psilocin.extraction.html
and it cannot be stressed enough, to extract from the basic phase asap, don't let it sit.
Click to expand...

Do you have to dephosphorylate psilocybin to extract via ion exchange resin? If yes, is there an easy way to add the phosphoryl group back on? I'm not sure that psilocin would survive vaporization. :(

That's a good study that you linked, I've read it before but I was looking for a different way to extract without needing to heat up (or synthesize for that matter) glacial acetic acid.
 
But I know from experience, some people in the Psilocin extraction thread too. Not for certain if it was Psilocybin since no analysis, but active smoked for sure.

Yes but dilute sulfuric would defeat the purpose. Needs to be concentrated to turn sugars to carbon.
 
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