METHOD FOR PREPARING D-BIOTIN

摘要

Abstract The invention discloses a D-biotin preparation method. In the prior art, with a synthesis method utilizing malonic acid diester as raw materials, impurities are also produced along with the obtained D-biotin. The D-biotin preparation method is characterized in that with the presence of dimethyl sulfoxide and inorganic base as catalysts, methane tricarboxylic acid trialkyl ester and (3aR, 8aS, 8bS)-1,3-dibenzyl-2-oxo-10H-iminazole [3,4-d] thiophene [1,2-a] sulfuryl halide are subjected to condensation reaction in methylbenzene solvent to obtain intermediate (3 aS,4S,6aR)- 1,3 -dibenzyl-4-(ω,ω,ω-3-methoxycarbonylbutyl)-4H- 1H-thiophene[3,4-d]iminazol e-2,4(1H)-ketone, and the D-biotin is obtained after the intermediate is treated by the aftertreatment method. By the D-biotin preparation method, production of the impurities is avoided, quality of the biotin is greatly improved on the existing basis, and side reaction is avoided too.

主权项

1. The D-biotin preparation method is characterized in that with the presence of catalysts including dimethyl sulfoxide and inorganic base, methane tricarboxylic acid trialkyl ester and compound formula B of (3aR, 8aS, 8bS)-1,3-dibenzyl -2-oxo-10H-iminazole [3,4-d] thiophene [1,2-a] sulfuryl halide are subjected to condensation reaction in methylbenzene solvent to obtain intermediate compound of formula A of (3 aS,4 S,6aR)-1,3-dibenzyl-4-(ω, ω, ω-3 -methoxycarbonylbutyl)-4H-1H-thiophene[3 ,4-d]iminazole-2,4(1H)-ketone and the D-biotin is obtained after the intermediate is treated by the aftertreatment method, wherein usage of the dimethyl sulfoxide is 5-10% of that of the methylbenzene solvent.