HRID651237

反应详情

EQUATION

反应方程式

HRID 651237 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 2,6-difluorobenzyl azide (34.2 g), 2-chloroacrylonitrile (17.73 9) and water (125 ml) is stirred at about 80° C. for 48 hours. Excess 2-chloroacrylonitrile is distilled off by raising the external temperature to about 130° C. The semi-solid mixture is cooled to about 40° C. and the suspension is treated with cyclohexane (50 ml), brought to about 20° C. and stirred for about 2 hours. The product is isolated by filtration, washed with cyclohexane (75 ml) and then with water and dried in vacuo at about 60° C.

WORKUP

后处理

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