HRID644502

反应详情

EQUATION

反应方程式

HRID 644502 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 7-amino-1-phenyl-5-trifluoromethylbenzimidazole (300 mg, 1 mmol), benzoylchloride (0.23 ml, 2 mmol) and triethyl amine (0.3 ml, 2 mmol) in tetrahydrofurane (10 ml) was stirred at ambient temperature overnight. The solvent was removed under reduced pressure and the residue was partitioned between ethyl acetate and hydro chloric acid (4M). The aqueous phase was rendered alkaline with saturated, aqueous sodium carbonate and extracted with ethyl acetate. The extract was dried and concentrated under reduced pressure and the resultant gum was triturated with a mixture of diethyl ether and petroleum ether to leave the solid, off-white product (145 mg, 38%), m/z, 382.1 (M+H)+.

WORKUP

后处理

  1. customThe solvent was removed under reduced pressure
  2. customthe residue was partitioned between ethyl acetate and hydro chloric acid (4M)
  3. extractionextracted with ethyl acetate
  4. customThe extract was dried
  5. concentrationconcentrated under reduced pressure
  6. customthe resultant gum was triturated with a mixture of diethyl ether and petroleum ether