HRID543333

反应详情

EQUATION

反应方程式

HRID 543333 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 6.4 g of 2-chloro-5-(1-imidazolyl)- 2',6'-dimethyl-4'-carboxybenzophenone and 0.8 g of sodium hydroxide in 35 ml of water is added 1.4 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 insoluble 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, washed with water and acetone and dried to give 6.1 g of α-(2,6-dimethyl-4-carboxyphenyl)-2-chloro-5-(1-imidazolyl)benzenemethanol, melting at 317°-320° C. with decomposition as white crystals.

WORKUP

后处理

  1. customAfter completion of the reaction
  2. filtrationa small amount of an insoluble substance is filtered off from the warm mixture
  3. stirringunder stirring at 80°-90° C
  4. filtrationThe precipitated crystals are collected by filtration under reduced pressure
  5. washwashed with water and acetone
  6. customdried