HRID1428992

反应详情

EQUATION

反应方程式

HRID 1428992 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Part A: To a magnetically stirred suspension of 2,5-dimethyl-1-phenyl-1H-imidazole-4-carboxylic acid (0.4 gram, 1.85 mmol) in CHCl3 (4 ml) was added oxalyl chloride (0.34 gram, 2.685 mmol) and the resulting mixture was reacted at 58° C. for 2 hours and subsequently concentrated in vacuo. The resulting residue was taken up in dichloromethane and diisopropylethylamine (0.28 gram, 2.148 mmol) was subsequently added. A solution of 2,3-dichloroaniline (0.35 gram, 2.146 mmol) in dichloromethane (5 ml) was slowly added to the resulting mixture and the resulting mixture was reacted for 2 hours at room temperature and subsequently concentrated in vacuo. The resulting residue was purified by flash chromatography (dichloromethane) to give N-(2,3-dichlorophenyl)-2,5-dimethyl-1-phenyl-1H-imidazole-4-carboxamide (0.24 gram, 36% yield). Melting point: 127-129° C.

WORKUP

后处理

  1. customthe resulting mixture was reacted at 58° C. for 2 hours
  2. concentrationsubsequently concentrated in vacuo
  3. customthe resulting mixture was reacted for 2 hours at room temperature
  4. concentrationsubsequently concentrated in vacuo
  5. customThe resulting residue was purified by flash chromatography (dichloromethane)