反应详情

温度

110 °C

2 g (1 eq) of 3-methoxybenzamide was mixed with 3.1 ml (2.7 eq) of chloroacethylchloride and the resulting mixture was heated at 110° C. for 1 h. After cooling, the resulting solid was recrystallized in CHCl3. The resulting solid was added to a suspension of NaH (489 mg, 1.1 eq) in DME at 0° C. After 30 min, the resulting mixture was refluxed for 5 h, cooled to RT and hydrolyzed, extracted with AcOEt, washed with NaCl salt and dried. The resulting solid was recrystallized in a mixture hexane/AcOEt giving 16 as a white solid in 26% yield.

1. temperatureAfter cooling
2. customthe resulting solid was recrystallized in CHCl3
3. temperaturethe resulting mixture was refluxed for 5 h
4. temperaturecooled to RT
5. extractionhydrolyzed, extracted with AcOEt
6. washwashed with NaCl salt
7. customdried
8. customThe resulting solid was recrystallized in a mixture hexane/AcOEt giving 16 as a white solid in 26% yield