HRID647456

反应详情

EQUATION

反应方程式

HRID 647456 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

Cis-3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropane carboxylic acid (199 g, 0.95 M) was added to a solution of potassium carbonate (65.6 g, 0.475 M) in water (450 ml). Toluene (900 ml), tetra-n-butylammonium bromide (13.5 g, 0.05 M) and alpha-cyano-3-phenoxybenzyl p-toluenesulphonate (341 g, 0.9 M; prepared as described in A above) were added to the stirred mixture which was then heated at 70° C. for 3 hours. The mixture was cooled to ambient temperature and the organic phase was separated off, washed with aqueous potassium carbonate solution (2×200 ml) and water (2×200 ml), evaporated and degassed under vacuum to leave cis-alpha-cyano-3-phenoxybenzyl 3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropanecarboxylate as a pale amber oil (364 g, 97.3%), containing less than 1% trans-isomers.

WORKUP

后处理

  1. customprepared
  2. additionwere added to the stirred mixture which
  3. temperatureThe mixture was cooled to ambient temperature
  4. customthe organic phase was separated off
  5. washwashed with aqueous potassium carbonate solution (2×200 ml) and water (2×200 ml)
  6. customevaporated
  7. customdegassed under vacuum