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freeze precip of psilocin

Migrated topic.
Yes, I tested a small ammount. Was essentially tasteless. I feel it was beyond placebo. Matches what the mass spectra says.

Need to make more and reproduce/refine further. If yields are descent I think this could be practical one day. One promising thing is that the fumarate seems very stable and does not change color, which has happened before to me with other mushroom extract approaches.
 
Update is that yields have been low. This is dissapointing because we did finally did get psilocin fumarate.

There may be a loss when changing the pH or during other steps, I don't know.

Because of these issues, to make a practical extract I'll be working with ion resins next in the thread that Benz started.
 
Loveall said:
Update is that yields have been low. This is dissapointing because we did finally did get psilocin fumarate.

There may be a loss when changing the pH or during other steps, I don't know.

Because of these issues, to make a practical extract I'll be working with ion resins next in the thread that Benz started.
Click to expand...

Isn't the problem here that you are making a Calcium Hydroxide paste with a high pH of 12? That is destroying nearly all the compounds.

From what I have gathered it seems like the best bet for isolated actives is following this procedure to a T; aside from substituting diethyl ether with DCM and fiddling with the base titration compounds.

"A representative sample of 2 to 10g of dried 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."

If you can't evap under nitrogen I would back extract with ascorbate solution of pH4 multiple times and then air temp evap with a fan.
 
Scylla said:
Loveall said:
Update is that yields have been low. This is dissapointing because we did finally did get psilocin fumarate.

There may be a loss when changing the pH or during other steps, I don't know.

Because of these issues, to make a practical extract I'll be working with ion resins next in the thread that Benz started.
Click to expand...

Isn't the problem here that you are making a Calcium Hydroxide paste with a high pH of 12? That is destroying nearly all the compounds.

From what I have gathered it seems like the best bet for isolated actives is following this procedure to a T; aside from substituting diethyl ether with DCM and fiddling with the base titration compounds.

"A representative sample of 2 to 10g of dried 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."

If you can't evap under nitrogen I would back extract with ascorbate solution of pH4 multiple times and then air temp evap with a fan.
Click to expand...

Yeah, that's Casale's lab method (1985), we've posted that before. Diethyl ether and nitrogen evap are not easily available.

I got some mushrooms with some rust spots which I don't want to use. I'm gonna burn them
in an experiment.

- Dry and grind to a powder
- Make a water paste with ascorbic acid, and heat to 70C to try to convert to psilocin
- Add excess sodium bicarbonate (pH should be 8 ), quickly extract with ethyl acetate
- Add ~10mg/g of citric acid to ethyl acetate extract, see if clouds form and precipitate
 
I feel the need to contribute to this project. I am very close to getting this method up and running (UHPLC-CAD), and it is amenable to characterizing counterions and analytes, unlike LCMS and HPLC-UV. Loveall, I will accept samples, on the house, to generate data for this project. I reiterate...I don't want compensation.
It is certainly worth the effort, and there is no data/study to elucidate. It would quite literally, be the only data in the world, using this method.
 
Thanks benzyme.

I did a test run and got clouding and precipitation after salting the EA. Kind of cool. I tested a small amount of what crashed. I think I felt something, but can say it's beyond placebo.

Definitely worth doing more tests in my opinion.
 
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