HRID1387148

反应详情

EQUATION

反应方程式

HRID 1387148 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5 mmol of diphenyl N-cyanocarbonimidate are stirred with 5 mmol of cyclohexylmethylamine in 20 ml of acetonitrile for 2 h at room temperature. 5 mmol of 3-(1H-imidazol-4-yl)propanamine are then added and the mixture is brought to reflux for 8 h. The solution is concentrated under vacuum until dryness and the residue taken up in 5% acetic acid and washed with diethyl ether. After having been basified, the solution is extracted several times with dichloromethane. The combined and concentrated organic phases are purified by chromatography. The title compound is obtained, after concentration, in the form of a dry foam from diethyl ether.

WORKUP

后处理

  1. temperatureto reflux for 8 h
  2. concentrationThe solution is concentrated under vacuum until dryness
  3. washwashed with diethyl ether
  4. extractionthe solution is extracted several times with dichloromethane
  5. customconcentrated organic phases are purified by chromatography