HRID1454360

反应详情

EQUATION

反应方程式

HRID 1454360 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
9 °C

PROCEDURE

实验过程

50 g of donepezil was dissolved by stirring in 240 g of ethanol under heating, followed by adding 15.1 g of concentrated hydrochloric acid thereto at the internal temperature of 30° C. Then, it was cooled and continued stirring while keeping the internal temperature at about 25° C. Crystals started precipitating about 1 hour after the concentrated hydrochloric acid was poured into the mixture. After the precipitation started, the mixture was stirred at the internal temperature of 25° C. for 17 hours and then cooled to the internal temperature of 9° C. The crystals were collected by filtration and dried about 3 hours after the cooling was started, to give 52.25 g of polymorphic crystal (III) of donepezil hydrochloride (yield: 95.3%).

WORKUP

后处理

  1. temperatureunder heating
  2. customat the internal temperature of 30° C
  3. temperatureThen, it was cooled
  4. customat about 25° C
  5. customCrystals started precipitating about 1 hour after the concentrated hydrochloric acid
  6. additionwas poured into the mixture
  7. customAfter the precipitation
  8. stirringthe mixture was stirred at the internal temperature of 25° C. for 17 hours
  9. filtrationThe crystals were collected by filtration
  10. customdried about 3 hours after the cooling