HRID904749

反应详情

EQUATION

反应方程式

HRID 904749 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

24.7 g. of 2,2-dimethyl-3-(2,2-dichlorovinyl)-cyclopropane-1-carboxylic acid ethyl ester (purity: 96%, cis)trans ratio: 40:60), 6.7 g. of a 30% aqueous potassium hydroxide solution and 0.05 g. of polyoxyethylenesorbitane monooleate are stirred at 70° C. for 60 minutes. Stirring is continued with a further 6-g. portion of the potassium hydroxide solution for 60 minutes and with an additional 6-g. portion for 120 minutes. The solution is diluted with 100 ml. of water and 40 ml. fraction is distilled off to remove volatile, non-hydrolyzed substances. To the residual aqueous solution 80 cm3 of hexane is added followed by the addition of 12 g. of a 36% aqueous hydrochloric acid solution at 60° C. with stirring. The reaction mixture is then further manufactured as described in Example 1. 19.8 g. (95%) of 2,2-dimethyl-3-(2,2-dichlorovinyl)cyclopropane-1-carboxylic acid are obtained. Cis/trans ratio: 40:60.

WORKUP

后处理

  1. additionThe solution is diluted with 100 ml
  2. distillationfraction is distilled off
  3. customto remove volatile
  4. additionTo the residual aqueous solution 80 cm3 of hexane is added
  5. additionfollowed by the addition of 12 g
  6. stirringof a 36% aqueous hydrochloric acid solution at 60° C. with stirring