HRID2285663

反应详情

EQUATION

反应方程式

HRID 2285663 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

31 g (0.2 mole) of 3,3-dimethyl-pent-4 -enoic acid, N,N-dimethylamide are added dropwise, in the course of 3 hours, to a solution of 1 g of azo-bis-isobutyronitrile in 308 g (2 moles) of carbon tetrachloride at 75°-80° C. The mixture is stirred for 1.5 hours at 75°-80° C., a further 1 g of azo-bis-isobutyronitrile is added, and the temperature is maintained for a further 2 hours. After distilling off the unconverted starting materials at a bath temperature not exceeding 150° C., a residue is left, and this is stirred with 100 ml of water at 80°-90° C. for 1 hour. 17 g (0.08 mole) of 5-(2,2-dichlorovinyl)-4,4-dimethyl-tetrahydrofuran-2-one are thereby obtained as a water-insoluble phase.

WORKUP

后处理

  1. temperaturethe temperature is maintained for a further 2 hours
  2. distillationAfter distilling off the
  3. customexceeding 150° C.
  4. waita residue is left
  5. stirringthis is stirred with 100 ml of water at 80°-90° C. for 1 hour