HRID2285662

反应详情

EQUATION

反应方程式

HRID 2285662 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 40 g (0.26 mole) of 3,3-dimethylpent-4-enoic aicd N,N-dimethylamide, 231 g (1.5 moles) of carbon tetrachloride and 7 g (0.05 mole) of di-tert.-butyl peroxide is stirred for 6 hours at 140° C. in a stainless steel autoclave. 180 g (1.17 mole) of carbon tetrachloride are then distilled from the reaction mixture under reduced pressure, and the residue is stirred with 200 g of water for 1 hour at 80°-90° C. Extraction with methylene chloride, and subsequent distillation of the methylene chloride solution, gives 39 g (0.19 mole) of 5-(2,2-dichlorovinyl)-4,4-dimethyltetrahydrofuran-2-one, of boiling point 101° C./0.27 mbar.

WORKUP

后处理

  1. extractionExtraction
  2. distillationwith methylene chloride, and subsequent distillation of the methylene chloride solution