反应详情

温度

80 °C

A mixture of 2,6-difluorobenzyl azide (34.2 g) and 2-chloroacrylonitrile (26.6 g) is stirred at about 80° C. for 24 hours. n-Heptane (125 ml) is allowed to run in, and unreacted 2chloroacrylonitrile and 2,6-difluorobenzyl azide as well as n-heptane are distilled off (distillate 50 ml) by raising the external temperature to about 130° C. The mixture is cooled to about 20° C. and the suspension is stirred at about 20° C. for 1 hour. The product is isolated by filtration and washed with n-heptane (100 ml). The product is dried in vacuo at about 60° C. Yield: 31.55 g=71.6% (beige powder).

1. distillationare distilled off (distillate 50 ml)
2. temperatureby raising the external temperature to about 130° C
3. temperatureThe mixture is cooled to about 20° C.
4. stirringthe suspension is stirred at about 20° C. for 1 hour
5. customThe product is isolated by filtration
6. washwashed with n-heptane (100 ml)
7. customThe product is dried in vacuo at about 60° C