反应详情

To a solution of morpholine (11 g, 126.44 mmol, 2.01 equiv) in dichloromethane (60 mL) 0˜5° C. was added a solution of 3-(4-bromophenyl)propanoyl chloride (15.5 g, 63.01 mmol, 1.00 equiv) in dichloromethane (30 mL) dropwise with stirring. The resulting solution was stirred at 0˜5° C. for 1 h. The reaction mixture was warmed to room temperature. The resulting solution was diluted with 40 mL of water. The mixture was extracted with dichloromethane 2×100 mL. The combined organic layers was washed with 3×50 mL of brine, dried over anhydrous sodium sulfate and concentrated under vacuum to give 17.4 g (93%) of 3-(4-bromophenyl)-1-morpholinopropan-1-one as a white solid.

1. stirringThe resulting solution was stirred at 0˜5° C. for 1 h
2. extractionThe mixture was extracted with dichloromethane 2×100 mL
3. washThe combined organic layers was washed with 3×50 mL of brine
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated under vacuum