My Russian isn't what it used to be anymore
, but here is a translation of Dennis_pro's post:
(I'll include the pictures too)
dennis_pro(HyperLab Bee)
05-26-04 05:23
Post 509654 (missing)
(dennis_pro: "Èëëþñòðèðîâàííîå äåêàðáîêñèëèðîâàíèå", Russian HyperLab)Illustrated decarboxylation(Rated as: excellent)
As the catalyst was used menthone, which was obtained by the oxidation of menthol using potassium dichromate in the presence of sulfuric acid, employing the general procedure as described in Organikum.
20 g DL- tryptophan was placed into the flask, equipped with a reflux condenser and stirrer
(? don't see one on the pictures -VV) , and there was added 50 ml of dimethylsulfoxide (pharmaceutical grade "dimexid"), followed by a solution of 0.5 ml menthone in 5 ml of acetone, and, using good stirring (caution: evolution of carbon dioxide, strong frothing!) was heated to 150-180°C for an hour (actually the reaction already subsided after 30 min).
(That last part of the sentence, is that correctly translated? "??? 150-180? ? ? ?"))
30 minutes after the reaction started boiling, there was added through the condensor 5 additional ml of acetone (the vapors of acetone protect the reaction mixture from oxidation by atmospheric oxygen). When the reaction was finished, the solution became completely transparent and the evolution of carbon dioxide ceased.
The resulting pink coloured solution was allowed to cool and was diluted with 200 ml water, causing the mixture to become cloudy and the base of tryptamine is liberated in the form of a red oil.
70% acetic acid was added which led to the complete dissolution of oil. This was neutralized with sodium bicarbonate until no more CO
2 was evolved. This caused part of resins to float together with the foam. The mixture was filtered through cotton, which removed floating resins. Nevertheless, the solution remained a red color. For a more complete removal of resins the mixture was washed with a small quantity of dichloromethane.
Aqueous NaOH was added, which caused the mixture to become cloudy, and after standing overnight tryptamine precipitated, which was filtered off and dried. Tryptamine obtained this way will still contain traces of NaOH. Attempts at washing the precipitate on the filter with water will lead to the significant losses of tryptamine as a result of its significant solubility in the water (34 g/l).
Since tryptamine possesses significant solubility in the water, it is better to extract the resulting alkaline suspension of tryptamine three times with benzene. Extracts are pooled and dried with anhydrous MgSO
4, and to this is added just enough petroleum ether to turn the solution cloudy, and the solution is left overnight in the refrigerator. During the night tryptamine is crystallized in the form of completely colorless needles.
/
zavtra I will report this
fotku, forgot
krassota / The general output not of
schitan, since with the experiments separation of candy (tryptamine) from
govna resin) product threw out itself on
nemnogu into the toilet. Procedure will be improved on the following week, with the application of the almost inert gas:)
P.S. The use of the organic
(?) solvents, acetic acid and bicarbonate is compulsory, an attempt at the acidification by sulfuric acid, and the extraction of resin by petroleum ether did not succeed, since resins and tryptamine in it were left mostly undissolved.
Attempts to directly basify the solution and to immediately extract tryptamine with benzene lead to the isolation of red noncrystallizing resin: