反应详情

温度

80 °C

A mixture of 2,6-difluorobenzyl azide (34.2 g), 2-chloroacrylonitrile (26.6 g) and n-heptane (125 ml) is stirred at about 80° C. for 24 hours, whereby a suspension results. Unreacted 2-chloroacrylonitrile and 2,6-difluorobenzyl azide as well as n-heptane are distilled off (distillate 25 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 about 2 hours. The product is isolated by filtration, washed with n-heptane (100 ml) and dried in vacuo at about 60° C. Yield: 20.45 g=46.4% (beige powder).

1. customwhereby a suspension results
2. distillationare distilled off (distillate 25 ml)
3. temperatureby raising the external temperature to about 130° C
4. temperatureThe mixture is cooled to about 20° C.
5. stirringthe suspension is stirred at about 20° C. for about 2 hours
6. customThe product is isolated by filtration
7. washwashed with n-heptane (100 ml)
8. customdried in vacuo at about 60° C