Sodium Hydroxide → Y-20811 free acid

Participants

Reaction Steps

To a solution of 16.2 g of 2-methyl-5-(1-imidazolyl)-2',6'-dimethyl-4'-carboxybenzophenone and 2.1 g of sodium hydroxide in 113 ml of water is added 2.8 g of sodium borohydride, and the mixture is stirred at 70°-75° C. for 3 hours. After completion of the reaction, a small amount of an isoluble substance is filtered off from the warm mixture and the filtrate is adjusted to pH 4 with concentrated hydrochloric acid under stirring at 80°-90° C. The precipitated crystals are collected by filtration under reduced pressure and washed with water well. After drying, recrystallization from dimethylformamide gives 14.0 g of α-(2,6-dimethyl-4-carboxyphenyl)-2-methyl-5-(1-imidazolyl)benzenemethanol, melting at 310°-312° C. with decomposition.

Provenance & Evidence