HRID647808

反应详情

EQUATION

反应方程式

HRID 647808 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.9 g (28.1 millimoles) of 1-chlorocyclopropanecarboxylic acid chloride are added, with stirring, to 4.5 g (23.3 millimoles) of 3-(p-aminobenzoyl)-propionic acid in 100 ml of absolute tetrahydrofuran. The reaction mixture is then stirred for 20 hours at room temperature, followed by 7 hours under reflux. A small amount of solid is filtered off and discarded, and the filtrate is concentrated. The residue obtained is recrystallized from ethyl acetate, giving 3.4 g (49% of theory) of 3-[p-(1-chlorocyclopropylcarbonylamino)-benzoyl]-propionic acid as colorless crystals, of melting point 178°-179° C.

WORKUP

后处理

  1. waitfollowed by 7 hours
  2. temperatureunder reflux
  3. filtrationA small amount of solid is filtered off
  4. concentrationthe filtrate is concentrated
  5. customThe residue obtained
  6. customis recrystallized from ethyl acetate