HRID894295

反应详情

EQUATION

反应方程式

HRID 894295 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a chilled suspension of zinc powder (0.494 g, 0.0076 mole) in 0.57 ml of acetic acid and 3 ml of ether was added dropwise over a period of 20 minutes a solution of 4-tribromomethyl-6,6-dimethyl-2-oxo-3-oxabicyclo[3.1.0]hexane (0.72 g, 0.0019 mole) in 5 ml of ether. The mixture was stirred at 0° for one hour. After adding 30 ml of ether and 5 ml of water, the mixture was filtered through Celite filter aid. The organic layer was separated, washed three times with saturated aqueous sodium chloride, dried over magnesium sulfate, and the ether was removed by evaporation to give crystalline cis-3-(2,2-dibromovinyl)-2,2-dimethylcyclopropanecarboxylic acid (0.489 g, 86% yield); mp, 112°-114° after recrystallization from n-hexane.

WORKUP

后处理

  1. filtrationthe mixture was filtered through Celite
  2. filtrationfilter aid
  3. customThe organic layer was separated
  4. washwashed three times with saturated aqueous sodium chloride
  5. dry with materialdried over magnesium sulfate
  6. customthe ether was removed by evaporation