HRID1731312

反应详情

EQUATION

反应方程式

HRID 1731312 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

0.5 mol of sodium 4-chlorophenolate in acetonitrile are added dropwise to a solution of 125 g (1 mol) of 3-chloro-2-chloromethylpropene in 50 ml of acetonitrile. After addition of 0.5 g of sodium iodide, the reaction mixture is heated under reflux for 12 hours and is then filtered cold. The filtrate is concentrated in vacuo. The residue is dissolved in methylene chloride and the solution is washed with water, dried over sodium sulphate and concentrated. 58.6 g of about 60% pure 2-chloromethyl-3-(4-chlorophenoxy)-propene are obtained and are dissolved in 500 ml of methylene chloride, and 43 g (0.25 mol) of 3-chloroperbenzoic acid are added.

WORKUP

后处理

  1. temperaturethe reaction mixture is heated
  2. temperatureunder reflux for 12 hours
  3. filtrationis then filtered cold
  4. concentrationThe filtrate is concentrated in vacuo
  5. dissolutionThe residue is dissolved in methylene chloride
  6. washthe solution is washed with water
  7. dry with materialdried over sodium sulphate
  8. concentrationconcentrated