HRID35220

反应详情

EQUATION

反应方程式

HRID 35220 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of β-(3,4-dimethoxyphenyl)ethylamine (100 g, 0.552 m) and triethylamine (66.6 g, 0.66 m) in CHCl3 (1 liter) was added acetyl chloride (47.1 g, 0.60 mole) dropwise over a period of 30 min. and the mixture stirred overnight. The mixture was washed with 3×500 ml H2O, dried over MgSO4 and evaporated to a solid. The solid was dissolved in 500 ml hot CCl4, 300 ml cyclohexane added and allowed to cool slowly. The crystallized solid was collected by filtration and dried to afford N-acetyl-3,4-dimethoxyphenethylamine as a white solid, 112.1 g (91% yield). m.p. 99°-100°.

WORKUP

后处理

  1. washThe mixture was washed with 3×500 ml H2O
  2. dry with materialdried over MgSO4
  3. customevaporated to a solid
  4. dissolutionThe solid was dissolved in 500 ml hot CCl4
  5. addition300 ml cyclohexane added
  6. temperatureto cool slowly
  7. filtrationThe crystallized solid was collected by filtration
  8. customdried