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
- 32.5 °C
PROCEDURE
实验过程
A 250 ml flask equipped with overhead stirrer and gas inlet was charged with 34 g of bupropion base and 138 ml of isopropanol. The solution was maintained under stirring while 13 g of gaseous HBr was introduced through the gas inlet in a time of 20′ while the internal temperature of the mixture raises from 25 to 40° C. During the gas addition a heavy white precipitate formed. At the end of the gas addition the temperature of the mixture was raised to reflux (80° C.), to get complete solution of the suspended solid. The temperature was then lowered to 25° C. in 1 hour and further lowered to 0-5° C. in 1 additional hour. The precipitate obtained was filtered and washed with 20 ml of cold isopropanol. The discharged wet solid was dried under vacuum (30 mmHg) in a static drier at 50° C. for 16 hours. 34 g of bupropion hydrobromide form I were obtained.
WORKUP
后处理
- customA 250 ml flask equipped with overhead stirrer and gas inlet
- temperatureThe solution was maintained
- additionDuring the gas addition a heavy white precipitate
- customformed
- additionAt the end of the gas addition the temperature of the mixture
- temperaturewas raised
- temperatureto reflux (80° C.)
- customto get complete solution of the suspended solid
- customfurther lowered to 0-5° C. in 1 additional hour
- customThe precipitate obtained
- filtrationwas filtered
- washwashed with 20 ml of cold isopropanol
- customThe discharged wet solid was dried under vacuum (30 mmHg) in a static drier at 50° C. for 16 hours