I think the described simple soxhlet method indeed produces big transparent crystals. But they are of urea, not psilocybin. If I am correct (lilienthal feel free to correct me), the urea is the first alkaloid which is taken up by the condensed (no longer boiling) 190 proof ethanol in the soxhlet tube, and it is the last crystal which precipitates in the collected solvent.
I have a nice jpg of the large (half inch) urea crystals which were obtained with a simple soak for 5 minutes at roomtemperature in 96 percent ethanol.
(what was extracted was the residue which remained after the extraction of cubensis powder in 140 proof ethanol (of pH3 with HCl), evap down, cleaning with pet ether and acetone)
The residue was washed twice with cold 190 proof (96 percent) ethanol. The first wash made the ethanol yellowish, the 2nd wash remained transparent.
The solvent was removed from the residue by use of a balloon pipette, chilled to minus tenty centigrade (after soaking) for about 12 hours. Tiny crystals formed. Then the solvent was placed at roomtemperature again and the yellowish transparentcrystals grew over a period of three days (still submerged in 96 percent ethanol).
Then the crystals were filtered out, dried, photographed and placed in an oven. They melt somewhere between 150 and 160 centigrade. After cooling down, all what remains is a tiny bit brownish foam. Crystals are gone.
Unfortunately I do not have a website to link to, so if this forum is interested in the photo of the crystals please describe another way to post it (I can reduce the pic to less than 50Kb).
White (probably psilocybin hcl) crystals were obtained after the cold ethanol wash of the residue: the residue was extracted with boiling 190 proof ethanol. The ethanol was removed with a pipette and cooled to 4 centigrade. Then it went milky white. The dust-fine crystals showed an orange color reaction with freshly prepared Marquis reagent.
The lesson which I have learned today - again please correct me if I am wrong - is that it is really easy to get fooled when you try to obtain pure alkaloids from mushrooms. The nice big transparent crystals which are so easily obtained are of urea.
But urea is simple to recognize. If the mushroom extract is acidified with HCl, all alkaloids which crystallize from it are HCl salts. Urea HCl is yellowish, no matter how many times it is cleaned with something nonpolar. Psilocybin crystals are white.
