反应详情

温度

35 °C

940 ml of DMF dimethyl acetal are added to a solution of 200 g of 4-methylnicotinonitrile in 940 g of DMF, and the mixture is heated under reflux at 120-110 for 3 days. The mixture is cooled to 35° C., poured into 10 liters of ice-water and cooled at 4° C. for 16 h. The precipitate is filtered off, washed with water and dried, giving 263 g of 4-((E)-2-dimethylaminovinyl)nicotinonitrile; M˜173.22 g/mol; M+H found 174, NMR corresponds.

1. temperaturethe mixture is heated
2. temperatureunder reflux at 120-110 for 3 days
3. temperaturecooled at 4° C. for 16 h
4. filtrationThe precipitate is filtered off
5. washwashed with water
6. customdried