HRID1512196

反应详情

EQUATION

反应方程式

HRID 1512196 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

70 g (352.4 mmol) of methyl 4-(2-chloroethyl)benzoate [CAS Reg. No. 65787-72-6] and 146.2 g (880.9 mmol) of potassium iodide are suspended in 800 ml of acetonitrile and stirred under reflux for three days. After the reaction has gone to completion, the reaction solution is cooled and filtered, and the filtrate is evaporated to dryness under reduced pressure. The resulting residue is purified by flash chromatography on silica gel (mobile phase: petroleum ether/ethyl acetate 30:1→20:1). This gives 101 g (348.3 mmol, 98.8% of theory) of a yellowish oil.

WORKUP

后处理

  1. temperatureunder reflux for three days
  2. temperaturethe reaction solution is cooled
  3. filtrationfiltered
  4. customthe filtrate is evaporated to dryness under reduced pressure
  5. customThe resulting residue is purified by flash chromatography on silica gel (mobile phase: petroleum ether/ethyl acetate 30:1→20:1)