反应详情

温度

70 °C

A mixture of 2,6-difluorobenzyl azide (34.2 9), 2-chloroacrylonftrile (26.6 g) and water (125 ml) is stirred at about 70° C. for 24 hours. Excess 2-chloroacrylonitrile is distilled off by raising the external temperature to about 130° C. The mixture is cooled to about 95° C. and the product is crystallized by seeding. After cooling to about 40° C., the suspension is treated with cyclohexane (50 ml) and brought to about 20° C., and the product is isolated by filtration, washed with cyclohexane (75 ml) and then with water and dried in vacuo at about 60° C. Yield: 36.38 g=82.6%.

1. distillationExcess 2-chloroacrylonitrile is distilled off
2. temperatureby raising the external temperature to about 130° C
3. temperatureThe mixture is cooled to about 95° C.
4. customthe product is crystallized
5. temperatureAfter cooling to about 40° C.
6. additionthe suspension is treated with cyclohexane (50 ml)
7. custombrought to about 20° C.
8. customthe product is isolated by filtration
9. washwashed with cyclohexane (75 ml)
10. dry with materialwith water and dried in vacuo at about 60° C