反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureunder heating
- customat the internal temperature of 30° C
- temperatureThen, it was cooled
- customat about 25° C
- customCrystals started precipitating about 1 hour after the concentrated hydrochloric acid
- additionwas poured into the mixture
- customAfter the precipitation
- stirringthe mixture was stirred at the internal temperature of 25° C. for 17 hours
- filtrationThe crystals were collected by filtration
- customdried about 3 hours after the cooling