反应详情

温度

82 °C

A mixture of 2,6-difluorobenzylazide (9,22 g), 2-chloroacryonitrile (6,68 g) and water is stirred at about 82° C. for about 24 hours. 2-Chloroacrylnitrile is distilled off by raising the external temperature to about 113° C. excess. The mixture is cooled to about 40° C. and toluene (10 ml) is added. Within about 40 minutes at about 80° C. sodium hydroxide (5,5 ml—30%) is added the amide being crystallized. By raising the external temperature to 112° C., toluene is distilled off. The suspension is cooled to 20° C. and the product is isolated by filtration, washed with water (200 ml) and dried at about 60° C. in vacuo.

1. distillation2-Chloroacrylnitrile is distilled off
2. temperatureby raising the external temperature to about 113° C. excess
3. temperatureThe mixture is cooled to about 40° C.
4. additiontoluene (10 ml) is added
5. additionWithin about 40 minutes at about 80° C. sodium hydroxide (5,5 ml—30%) is added the amide being
6. customcrystallized
7. temperatureBy raising the external temperature to 112° C.
8. distillationtoluene is distilled off
9. temperatureThe suspension is cooled to 20° C.
10. customthe product is isolated by filtration
11. washwashed with water (200 ml)
12. customdried at about 60° C. in vacuo