HRID904748

反应详情

EQUATION

反应方程式

HRID 904748 的结构方程式

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

36.2 g. of 2,2-dimethyl-3-(2,2-dibromovinyl)-cyclopropane-1-carboxylic acid ethylester (purity: 90%, cis) trans ratio: 45:65/, 4 g. of a 25% aqueous sodium hydroxide solution and 0.2 g. of tricaprylmethyl ammonium chloride are stirred at 100° C. for 30 minutes, whereupon three 4-g. portions of the sodium hydroxide solution are added in 30 minutes intervals and stirring is continued for altogether 240 minutes. The mixture is cooled to 20° C., diluted with 100 ml. of water and extracted with 10 ml. of benzene. The aqueous solution is admixed with 12 g. of a 36% aqueous hydrochloric acid solution at 70° C. and cooled to room temperature with stirring. The precipitated acid is dissolved in 60 ml. of benzene, the solution is separated and the solvent is evaporated. 30.0 g (92%) of 2,2-dimethyl-3-(2,2-dibromovinyl)-cyclopropanecarboxylic acid are obtained. Cis/trans ratio: 40:60.

WORKUP

后处理

  1. additiondiluted with 100 ml
  2. extractionof water and extracted with 10 ml
  3. temperatureof a 36% aqueous hydrochloric acid solution at 70° C. and cooled to room temperature
  4. stirringwith stirring
  5. dissolutionThe precipitated acid is dissolved in 60 ml
  6. customof benzene, the solution is separated
  7. customthe solvent is evaporated