jim fear skrev:
Dextrose > Der var en post i svampeforummet om samme emne hvor du også snakker om acetat, men krydsposter lige mine betænkeligheder her:
Citat:
Jeg tror at du også vil få dannet en del 4-AcO-DMT hvis du bruger eddikesyre, da esterificeringen er syrekatalyseret. Tror jeg ville bruge HCl i stedet.
Hvis jeg skulle lave 4-AcO-DMT ville jeg bruge eddikesyre og en katalytisk mængde H2SO4, som normalt når man vil danne en ester.
Psilocybin bliver btw. nemt nedbrudt til psilocin, bla. ved opvarmning. Så det er temmelig sikkert psilocin du har hvis du har lavet fx. et varmt ethanol ekstrakt af svampe.
BTW så skriver Schulgin et sted at en blanding af ethanol og methanol skulle være det optimale opløsningsmiddel for psilocin.
Tjek det her link, af syntese af 4-AcO-DMT fumarat, som jeg skrev tror jeg der skal pænt meget mere en blot iseddike til at lave acetoxy-esteret.
http://psychedelichosting.info/Ionium/R ... cybin.htmlDen føromtalte extraktion er at finde her:
http://psychedelichosting.info/Ionium/R ... ction.htmlJeg citerer:
Citat:
This method permits rapid isolation of psilocin from hallucinogenic mushrooms by co-extraction of both psilocin and psilocybin. Dilute acetic acid is an excellent solvent for this purpose, because both compounds are very soluble in acetic acid and very little of other interfering substances are extracted, It is most likely some other compounds are co-extracted but are removed from psilocin in the ether extraction from the aqueous base. Psilocybin is completely dephosphorytated to psilocin by heating the acid extract. After addition of the base, extraction into ether should be performed promptly, because of decomposition of psilocin at a greater pH than 712. The extraction and dephosporylation steps produce reasonably pure psilocin from a small amount of mushroom material. Two grams of mushrooms will often be sufficient to obtain an infrared spectrum of psilocin (Fig. 1). Smaller mushrooms exhibits provide ample psilocin for mass spectral analysis (Fig. 2).
This method has been used in our laboratory for six months and has given excellent results in separating psilocin from methanol-soluble compounds. Other identification techniques such as gas chromatography and microcrystalline tests are possible on psilocin extracted by this method.
Godt nok bruger de ikke soxhlet i denne ekstraktion, som jeg også klart ville foreslå, men man kunne måske bruge deres fremgangsmåde, til at dephosporylere Psilocybinen i krystalmassen til Psilocin-acetat efter ekstraktionen med MeOH, som beskrevet i fremgangsmetoden citeret nedenunder:
Citat:
Experimental
A representative sample of 2 to 10g of dried mushrooms 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.
Crude psilocin will appear as a greenish residue. Recrystallization from chloroform/heptane (1:3) yields white crystals. The resulting powder can then be submitted to infrared and mass spectral analyses.
Som fremhævet nederst, ser det jo ud til at produktet Plutonium har fået er blandede psilocin/psilocybin alkaloider, men jeg foreslå at produktet får nogenlunde samme behandling som det jeg har fremhævet i citeringen.
Altså:
Opløs krystallerne til sidst i MeOH + overskud af ekv. iseddike, lad stå i en time, varm op til 70 grader (eller måske bare til MeOH's kogepunkt), og håb på at der udfælder Psilocin-acetat...?
Hvad syntes du, Plutonium? (Og andre?)
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