HRID1702922

反应详情

EQUATION

反应方程式

HRID 1702922 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 57 g trifluoroacetic acid and 105 g trifluoroacetic anhydride in 400 ml anhydrous acetonitrile are added dropwise to a stirred suspension of 95.1 g 3-(3-indolyl)propionic acid in 500 ml anhydrous acetonitrile and maintained with stirring at -15° for 30 minutes. Under good cooling 500 ml anhydrous pyridine are added between -20° and -15° and quickly 238 ml of a 4.2 N solution of anhydrous methylamine in acetonitrile. The mixture is warmed with stirring at 0° for 15 minutes and maintained to 0° for 3 hours. 3-(3-indolyl)-N-methyl-propionamide (M.pt 97°-98° after crystallization from methylene chloride/ethyl acetate) is obtained after working up.

WORKUP

后处理

  1. temperaturemaintained
  2. additionare added between -20° and -15°
  3. temperatureThe mixture is warmed
  4. stirringwith stirring at 0° for 15 minutes
  5. temperaturemaintained to 0° for 3 hours