HRID1709009

反应详情

EQUATION

反应方程式

HRID 1709009 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-bromo-1-(2,5-dimethoxyphenyl)-ethanone (10.0 g) is added dropwise to a solution of dimethylamine (6.1 g) in toluene (450 ml). The mixture is stirred overnight at room temperature and extracted with a 1-N water solution of hydrochloric acid (3×250 ml). The mixed aqueous phases are alcalinized with a 25% water solution of sodium hydroxide (200 ml) and extracted with dichloromethane (4×250 ml). The mixed organic phases are washed with water (3×200 ml) and dried over magnesium sulphate. The solvent is distilled in vacuo and the residue is dried in vacuo to constant weight to give 1-(2,5-dimethoxyphenyl)-2-dimethylamino-ethanone which is a liquid, b.p. 250°-255°.

WORKUP

后处理

  1. extractionextracted with a 1-N water solution of hydrochloric acid (3×250 ml)
  2. extractionextracted with dichloromethane (4×250 ml)
  3. washThe mixed organic phases are washed with water (3×200 ml)
  4. dry with materialdried over magnesium sulphate
  5. distillationThe solvent is distilled in vacuo
  6. customthe residue is dried in vacuo to constant weight