HRID428146

反应详情

EQUATION

反应方程式

HRID 428146 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Under argon, a solution of 2-(3,4-dimethoxyphenyl)-2-(methylthio)nitroethane (1.22 g, 4.8 mmol) in tetrahydrofuran (20 ml) was dropwise added to an ice-cooled and stirred solution of lithium aluminum hydride (0.47 g) in tetrahydrofuran (10 ml). After stirring at room temperature for 30 minutes, water (0.47 ml), 15% aqueous sodium hydroxide solution (0.47 g) and water (1.14 ml) were sequentially added dropwise to the reaction mixture under ice-cooling and stirring. A small amount of potassium carbonate was added and stirred for a few minutes. Inorganic salts were filtered out and washed with tetrahydrofuran and the filtrate was concentrated under reduced pressure and dried to yield a crude oily 2-(3,4-dimethoxyphenyl)-2-(methylthio)ethylamine (0.98 g).

WORKUP

后处理

  1. temperaturecooled
  2. temperaturecooling
  3. stirringstirring
  4. stirringstirred for a few minutes
  5. filtrationInorganic salts were filtered out
  6. washwashed with tetrahydrofuran
  7. concentrationthe filtrate was concentrated under reduced pressure
  8. customdried