HRID1631153
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
- 60 °C
PROCEDURE
实验过程
1 ml of 2-bromobenzaldehyde are dissolved in 20 ml of 1,2-dichloroethane and ml of tetrahydrofuran. 799 μl of cyclopropylamine and 643 μl of glacial acetic acid are added, and the mixture is stirred at 60° C. for 6 h. After cooling to 25° C., 5.3 g of sodium triacetoxyborohydride are added and stirred at 25° C. for a further 12 h. The mixture is poured into water, extracted three times with dichloromethane, and the combined organic phases are dried over sodium sulfate. After filtration, the filtrate is evaporated to dryness and purified by chromatography (reversed phase HPLC).
WORKUP
后处理
- temperatureAfter cooling to 25° C.
- stirringstirred at 25° C. for a further 12 h
- extractionextracted three times with dichloromethane
- dry with materialthe combined organic phases are dried over sodium sulfate
- filtrationAfter filtration
- customthe filtrate is evaporated to dryness
- custompurified by chromatography (reversed phase HPLC)