HRID980465

反应详情

EQUATION

反应方程式

HRID 980465 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

From 5.75 g (0.25 mole) of metallic sodium and 200 ml of methanol sodium methylate is prepared. 32 g (0.25 mole) of m-chloro-phenol are added, the mixture is refluxed for an hour and evaporated to dryness. The solid residue is suspended in 200 ml of benzene and 88 g (0.25 mole) of chloro acetonyl phosphorane are added. The reaction mixture is refluxed for 3 hours. The sodium chloride is removed by filtration of the hot mixture and the benzene filtrate is evaporated in vacuo. The residual solid crude product is rubbed with 50 ml of ether and the crystals formed are filtered and dried. Thus 97 g of the crystalline title compound are obtained, yield 87.2%.

WORKUP

后处理

  1. temperaturethe mixture is refluxed for an hour
  2. customevaporated to dryness
  3. temperatureThe reaction mixture is refluxed for 3 hours
  4. customThe sodium chloride is removed by filtration of the hot mixture
  5. customthe benzene filtrate is evaporated in vacuo
  6. customthe crystals formed
  7. filtrationare filtered
  8. customdried