HRID456985

反应详情

EQUATION

反应方程式

HRID 456985 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Donepezil oxalate (purified, example 2), 5 gms, was dissolved in water 50 ml under heating at 50° C. Stirring was continued for 1 hour with gradual cooling. At room temperature, dichloromethane 50 ml was added and stirred for 10 mins. Liquid Ammonia 5 ml was added slowly with stirring. The dichloromethane layer was separated and 50 ml water was added to it. Analytical grade concentrated hydrochloric acid 1.5 ml was slowly added and stirred for 10 mins. Dichloromethane was distilled off under vacuum at 45° C. to obtain Donepezil hydrochloride in water, which was kept for lyophilyzation for 24 hours at −35° C. to give Donepezil hydrochloride amorphous with a yield of 3.9 gms (95%).

WORKUP

后处理

  1. stirringstirred for 10 mins
  2. stirringwith stirring
  3. customThe dichloromethane layer was separated
  4. addition50 ml water was added to it
  5. additionAnalytical grade concentrated hydrochloric acid 1.5 ml was slowly added
  6. stirringstirred for 10 mins
  7. distillationDichloromethane was distilled off under vacuum at 45° C.