HRID428138

反应详情

EQUATION

反应方程式

HRID 428138 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To isopropanol (200 ml), 40% aqueous methylamine solution (133 ml) was added and stirred under ice-cooling. 2-Bromo-1-(3,4-dimethoxyphenyl)ethanone (8.47 g, 33 mmol) was dissolved in isopropanol (10 ml) and dichloromethane (10 ml) and dropwise added to the reaction mixture over 1 hour. After the dropwise addition, the mixture was stirred for 15 minutes under ice-cooling. The solvent in the reaction mixture was distilled out at room temperature under reduced pressure and the precipitated crystal was filtered to yield 1-(3,4-dimethoxyphenyl)-2-(methylamino)ethanone hydrobromide (6.36 g, 67%).

WORKUP

后处理

  1. temperaturecooling
  2. additionAfter the dropwise addition
  3. stirringthe mixture was stirred for 15 minutes under ice-
  4. temperaturecooling
  5. distillationThe solvent in the reaction mixture was distilled out at room temperature under reduced pressure
  6. filtrationthe precipitated crystal was filtered