反应详情

温度

100 °C

Diethylamine (180 mL) and triethylamine (90 mL) were added to a solution of 4′-bromo-4-chlorobutyrophenone (18.13 g) in acetonitrile (90 mL), and the mixture was stirred at 100° C. for one hour. The reaction solution was cooled to room temperature and water was added, followed by extraction with chloroform. The organic layer was dried over anhydrous magnesium sulfate and filtered. The solvent was then evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=5:1→ethyl acetate:methanol:triethylamine=40:4:1) to give 1-(4-bromophenyl)-4-(diethylamino)butan-1-one as a brown oil (9.02 g, 44%).

1. temperatureThe reaction solution was cooled to room temperature
2. extractionfollowed by extraction with chloroform
3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
4. filtrationfiltered
5. customThe solvent was then evaporated under reduced pressure
6. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=5:1→ethyl acetate:methanol:triethylamine=40:4:1)