HRID649628

反应详情

EQUATION

反应方程式

HRID 649628 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 120 ml of methanol solution containing 4.8 g of sodium hydroxide were added 11.1 g of 2,2-dimethyl-3-(2',2',2'-trichloroethyl)-cyclopropanecarboxylic acid (purity: 91.8%, cis/trans ratio: 82.8/17.2) to heat the resulting mixture for 37 hours under reflux. The mixture was diluted with water and neutral part was removed by extraction with ether. The water layer was acidified with conc. hydrochloric acid and extracted with ether. The ether layer was concentrated to obtain 8.15 g of 2,2-dimethyl-3-(2',2'-dichlorovinyl)-cyclopropanecarboxylic acid, cis/trans ratio 79.8/20.2, purity 92.4%, yield 86.8%.

WORKUP

后处理

  1. temperatureto heat the resulting mixture for 37 hours
  2. temperatureunder reflux
  3. customwas removed by extraction with ether
  4. extractionextracted with ether
  5. concentrationThe ether layer was concentrated