反应详情

温度

47.5 °C

(E)-3-(4-(Trifluoromethyl)phenyl)-2-propenoic acid (2400 g, 11.1 mol) and DMF (N,N-dimethylformamide)(82 ml) were added to toluene (12 L). SOCl2 (52.6 mL, 721 mmol) was added dropwise at room temperature and the mixture was stirred at 45-50° C. for 1 hour. The toluene solution cooled to room temperature was added dropwise to 25% aqueous ammonia (12L) at 5-25° C. The mixture was stirred at 45-55° C. for 1 hour. After allowing to cool to room temperature and stirring, the mixture was stirred at the same temperature for 1 hour. The precipitated crystals were collected by filtration, washed with water (12 L) and dried under reduced pressure to give (E)-3-(4-(trifluoromethyl)phenyl)-2-propenamide (2293 g, 10.7 mol, yield 96%).

1. stirringThe mixture was stirred at 45-55° C. for 1 hour
2. temperatureto cool to room temperature
3. stirringstirring
4. stirringthe mixture was stirred at the same temperature for 1 hour
5. filtrationThe precipitated crystals were collected by filtration
6. washwashed with water (12 L)
7. customdried under reduced pressure