HRID2050171

反应详情

EQUATION

反应方程式

HRID 2050171 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,500 ml of benzene was added to 1,423 g of N-(1'-hydroxy-2',2',2'-trichloroethyl)-2-hydroxy benzamide and then 833 g of thionyl chloride was added thereto and heated under reflux at 70°-80° C. for 4 hours to obtain N-(1',2',2',2'-tetrachloroethyl)-2-hydroxy benzamide (white crystal, melting point of 113°-113.5° C., Anal. Found: C,35.74; H,2.12; N,4.70 Calcd. for C9H7Cl4NO2 : C,35.68; H,2.33; N,4.62 and the resultant reaction mixture, without separation of the crystals, was cooled to below 30° C. and mixed with 1,250 g of methanol and heated under reflux for 2 hours at 55°-60° C. followed by removing the solvent and the residue was poured into water, filtered and dried to obtain 1,380 g (yield 92.4%) white crystals of N-(1'-methoxy-2',2',2'-trichloroethyl)-2-hydroxy benzamide.

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder reflux at 70°-80° C. for 4 hours