Blooming. 
11 Likes
What’s your process
Interesting thread, thank you everyone for contributing and showing your work; one of the best 500 post threads I’ve read in a while. 
Earlier I saw that people were using acetone to precipitate what I assume is the freebase form. I think a method that may be overlooked is salting the tryptamines to help drop the solubility in organic to increase both yield and purity, not to mention long-term stability.
The solubility of at least psilocybin in ethanol is low, dephosphorylated species like psilocin may have a bit more. Precipitating as an acidic salt will likely help the long-term stability and help drop the solubility in ethanol/acetone. I think something we are overlooking is the actual solubility of psilocybin in ethanol; it may be low, but even 5g/L can ruin yields since we are working in small quantities. I doubt it would gain solubility once it’s a salt, but it’s not uncommon to see organic cation/anion salt pairs lose water solubility and become more organic soluble when combined in solution; shit happens 
.
A seemingly preferable candidate for salting would be HCl as opposed to ascorbic acid since you would need much less to adjust pH and ascorbic acid is rather soluble in ethanol and acetone. This would also avoid the loss in solubility as mentioned above since HCl is a mineral acid.
I plan to do a few experiments playing with aqueous extractions at hot and cold temperatures with and without ultrasound, and under acidic conditions (all in a degassed environment). My reasoning for water opposed to ethanol/methanol due to all the impurities extracted and planning to precipitate more pure salts. I’m planning on experimenting with the acid (HCl vs acetic) and pH (1-4). The pKas listed for psilocybin are 10.3 for the amine, 6.5 and 1.3 for the phosphates, and -3 for the indole. With the ultrasonic, I’m expecting I can get away with less water, then I can use less solvent later to crash out tryptamine salts. Also, a pH around the pKa of the phosphate will likely help solubility, assuming dephosphorylation doesn’t occur at room temp.
I have a feeling that ethanol will be a better choice than acetone for purity’s sake because the other water-soluble components like sugar will have enough ethanol solubility to stay in solution whereas acetone would cause more impurities to precipitate; this would increase yield at the cost of purity, though it may increase stability.
I may also experiment with calcium salts at neutral or slightly basic pH to precipitate since calcium-phosphate bonds are preferred due to the hard-hard acid/base interaction. Calcium phosphate has low water solubility as is, without anything organic stuck to it.
If anyone has tried any of the above or thinks any of my reasoning is faulty, please tell me, especially with the extraction method, I figure a hot ultrasonic at neutral pH should work sufficiently well. I currently have no biological material at the moment to test this so I’m trying to use my expertise to make a plan before I possibly waste a bunch of material.
2 Likes
One more final step will be acetone crash.
If the goal is a Salt we need the free psilocin., Hcl and tartrate are write in the art. But Is more stable the psilocybin… the salt are more fast the efect… but is tricky the stabilization.
If you choose the hot acidic convert route for make a psilocin salt and work in a inert atmposhpere, and scavenger the O2 before the base step …is ok. The best solvent for the organic layer is Ethyl Acetate ,dyethyl ether or cloroform
And like i always says…for extractions and psilocin salts the best for me is Pan Cyan because the relation alkaloids and wheigt and garbages is the best.
1 Like
can’t salt PCB. can only salt psilocin to my knowledge.
also to add to what you were saying… the above acetone precip was a FASA after basifying (and doing lle). if you’re condensing ethanolic or methanolic extract , defatting then preciping. you’re precipitating sugars.
save the filtrate, condense and keep precipitating to keep removing sugar to end with a purer product.
4 Likes
occurs at room temp in any aqueous solution. over time is a given. but faster than you think. a week can be 50-90% loss according to lit.
then any added heat during solvent recovery will also slowly speed this up. you can easily oxidize a batch if you’re not being careful with aqueous extraction.
just use a different alcohol
2 Likes
I did some course predictions with solubilities of various calcium/magnesium chloride in ethanol, acetone and isopropanol, which have moderate solubility. But when cross-referencing with calcium/magnesium-phosphates (the tryptamine salt that would most resemble it), the water solubilities are very low in water, especially magnesium phosphates.
I have a feeling extracting neutrally at a pH of around 8.5 will yield highest water solubility allowing for the least amount of water to be used. Then the addition of CaCl2 or MgCl2 and cold temperatures could cause rather selective precipitation of PCB salts. I have to make sure this won’t do anything to the sugars, but at this pH, I doubt it.
It could very well be that the slight Lewis-acid character of the Mg2+ could catalyze dephosphorylation, but at least for isolation it would be helpful.
Adding something to scavenge radicals could really help the shelf-life dramatically as it’s at the very least oxidative degradation, if not photooxidation.
2 Likes
Metabisulfite for scavenge the o2
Din ligth after the basifyng step until the psilocin are salting helps to. Psilocin free is very sensitive to ligth and o2
After salting the best is put in a capsule in a glovebox or some edible that are traped and dont touch the air.
Psilocybin is much more stable.
After the acetone crash in the steps that i post before it can be crystalized in meoh.
1 Like
Aswome!! Love thats “shperulites”
1 Like
Interesting. It makes sense that aqueous environments would cause them to dephosphorylate due to the acidity of water helping catalyze and the general instability of phosphate esters.
By that logic, psilocybin is nearly impossible to stabilize. Seems like co-crystallized with sugar (acetone crash I presume) is actually a one of the better storage methods.
If the goal is to end up at psilocin for long-term storage, then absolute ethanol could be a good storage media because its likely soluble in ethanol.
1 Like
I’ve got a PowerPoint presentation I use to explain how CPC works that I would be glad to talk through. Offer stands for anyone else interested in learning in this thread.
6 Likes
I have some heptanol sitting around from the short time that I had a CPC. Never even got around to opening the bottle.
Just a thought. But you could extract in methanol preferably ultrasonic assisted. Dehydrate to a fine powder and run a continuous liquid extraction to defat. I’ve ran this apparatus in the past with DCM and the big issue was getting the drip rate perfect to much and you would flood, to little and the DCM droplets would stick to the powder and drag them to the bottom. It was nice because you could swing the pH in the vessel.
2 Likes
Yea my p. Tamps are actually Galindoi. Which Alan Rockerfellar (sp?) has recently sequenced the genome of, and established a new species. So right now p. Tampanesis, p. Galindoi, and p. Mexicana are our primary sclerotia producing species.
I’ve sampled my p. Galindoi, and a mild experience = ~ 5g dry… . an experience closer to an eighth of cubensis is ~10g dry sclerotia. 15 grams of dry sclerotia seems like it’d be a heavy dose, closer to 5grams of cubensis. I’ve never eaten fresh sclerotia, but 15grams is a typical strong dose in legal countries.
I don’t understand what this adaptogen tablet is… a complex of things?… a pressed pill of psilocybin? sorry if i missed it.
1 Like
Wild Bird Seed, Popcorn, and Oats.
Yea I’d have to make a water extract sludge… then a subsequent extract on that. or more.
I ended up bailing on the first attempt, I let the water sit out in a tub, assuming it would reduce quite a bit, but it did not. So I’m guessing a lot of my psilocybin was dephosphorylated by the time I reduced using heat. I’m not sure why I didn’t just boil the water down in the first place… Overall it was a big hassle and I’m having second thoughts about attempting it again. I am forsure leaving behind a significant ammount of actives in the media / sclerotia that are too small or brittle to harvest.
25 mg seems like the right dose! 
6 Likes
Still need to get some of those ordered.
4 Likes
I’ve been working too much to trip heavy