反应详情

温度

52 °C

To a suspension of 4′-acetamido-acetophenone 2 (21.84 g, 123 mmol) in acetic acid (184 mL), bromine (6.5 mL, 127 mmol) was added. The mixture was heated (inner temp: 52° C., oil bath temp: 60˜65° C.) with vigorous stirring until the suspension make a clear solution. The heating bath was rapidly removed, and the mixture was stirred at room temperature for 15 min and then stirred in an ice-water bath for 2 h(inner temp. 50° C.˜20° C.). The precipitation was filtrated, washed with 30% EtOH in water, and dried under reduced pressure to give 3 as a pale brown solid (24.0 g, 75% yield): MS(ES) m/e 257 [M+H].

1. additionwas added
2. customThe heating bath was rapidly removed
3. stirringthe mixture was stirred at room temperature for 15 min
4. stirringstirred in an ice-water bath for 2 h(inner temp. 50° C.˜20° C.)
5. customThe precipitation
6. filtrationwas filtrated
7. washwashed with 30% EtOH in water
8. customdried under reduced pressure