HRID848060

反应详情

EQUATION

反应方程式

HRID 848060 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10.3 g of a 20% acqueous NaOH solution was added dropwise to the mixture of 16.6 g of N-(1,2,2,2-tetrachloroethyl)-2-acetoxybenzamide, 70 ml of acetone and 5.3 g of phenyl mercaptan under stirring at 10°-15° C. The reaction was effected at room temperature for one hour. Water was added thereto, the dichloromethane layer was separated, and the solution was dried and concentrated. 100 ml of ethanol and 1.5 ml of 35% hydrochloric acid were added to the residue and the reaction was effected under reflux for two hours. The solvent was distilled off to obtain 14.5 g of N-(1-phenylthio-2,2,2-trichloroethyl)-2-hydroxybenzamide as white crystals.

WORKUP

后处理

  1. customthe dichloromethane layer was separated
  2. customthe solution was dried
  3. concentrationconcentrated
  4. addition100 ml of ethanol and 1.5 ml of 35% hydrochloric acid were added to the residue
  5. temperatureunder reflux for two hours
  6. distillationThe solvent was distilled off