HRID1283640

反应详情

EQUATION

反应方程式

HRID 1283640 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a cooled solution of 14.5 g. (0.078 mol.) of 3-chloro-4-hydroxybenzoic acid methyl ester and 4.0 g. (0.1 mol.) of sodium hydroxide in 100 ml. of water was dropwise added 9.8 g. (7.3 ml., 0.079 mol.) of dimethyl sulfate. The reaction mixture was refluxed for two hours. After cooling, ether was added and the layers were separated. The organic phase was washed with water, dilute sulfuric acid and water, dried (Na2SO4) and concentrated in vacuo to give 3-chloro-4-methoxybenzoic acid methyl ester, m.p. 72°-74°.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for two hours
  2. temperatureAfter cooling
  3. customthe layers were separated
  4. washThe organic phase was washed with water, dilute sulfuric acid and water
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated in vacuo