HRID1108904

反应详情

EQUATION

反应方程式

HRID 1108904 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3,4-dimethoxyphenylacetic acid (17.1 g, 0.090 mol) and carbonyldimidazole (14.6 g, 0.090 mol) in THF (200 ml) was stirred for 2.5 h in a flask fitted with a drying tube. To this solution was added 2-phenylethylamine (10.9 g, 0.090 mol) in THF (50 ml). After 1 h the THF was evaporated and the residue was treated with water (200 ml) and filtered. The crude amide was washed with water and recrystallized from mixture of 200 ml of methanol and 100 ml of water with a charcoal treatment to afford 21.6 g (80.3%) of the title compound mp 123°-124°. A second crop (2.1 g, (7.8%) was obtained after concentrating the mother liquors.

WORKUP

后处理

  1. customfitted with a drying tube
  2. customAfter 1 h the THF was evaporated
  3. additionthe residue was treated with water (200 ml)
  4. filtrationfiltered
  5. washThe crude amide was washed with water
  6. customrecrystallized from mixture of 200 ml of methanol and 100 ml of water with a charcoal treatment