FIELD: chemistry.
SUBSTANCE: described method relates to organic chemistry and specifically to a method of producing betulinic acid. Said method is realised as follows: before oxidation, betulin is dispersed in a donor coordinating solvent - acetone, preferably with exposure to ultrasound at frequency 20-50 kHz for 0.5-5.0 min, and then the betulin solution is mixed with a solution of a Keggin structure 12-heteropoly acid with content thereof in the reaction mixture of 1·10-5 -1·10-3 mol/l, wherein the heteropoly acids used are particularly tungstophosphoric acid (H3PW12O40) or molybdophosphoric acid (H7(P(Mo2O7)6) or molybdosilicic acid (H4(SiMo12O40) and a solution of a chromium (VI) compound, specifically: potassium dichromate (K2Cr2O7); oxidation of betulin is carried out for 60-240 min at temperature 15-35°C, and at the end of the oxidation reaction, the obtained betulonic acid is purified by separating the liquid phase containing betulonic acid from the residue and dilution thereof with water until a dispersion forms; the obtained dispersion is then filtered, the residue, which is betulonic acid, is washed with water, after which the betulonic acid is reduced with sodium borohydride in an organic solvent to betulinic acid. Output of the end product - betulinic acid - is equal to 88-92%.
EFFECT: method enables to achieve output of the end product - betulinic acid - of 88-92% with respect to the starting betulin, simple method and short implementation, as well as small volumes of organic solvents used and, as a result, realisation of the disclosed method virtually does not lead to environmental pollution.
5 cl, 3 ex, 1 tbl
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Authors
Dates
2012-08-20—Published
2011-05-10—Filed