HRID1172774

反应详情

EQUATION

反应方程式

HRID 1172774 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2.1 g (5.7 mmol) of N-[2-(4-bromophenylamino)phenyl]benzamide were suspended into 30 mL of xylene, 0.6 g (2.9 mmol) of p-toluenesulfonic acid monohydrate was added, and the whole was refluxed under heating for 3 hours. After the resultant had been stood to cool, the reaction solution was added with ethyl acetate, dichloromethane, and water for filtering insoluble matter out. An organic layer was extracted from a mother liquor, washed with water and a saturated sodium chloride solution, and dried with anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by means of silica gel column chromatography to obtain 1.0 g of 1-(4-bromophenyl)-2-phenyl-1H-benzimidazole (52% yield).

WORKUP

后处理

  1. additionwas added
  2. temperaturethe whole was refluxed
  3. temperatureunder heating for 3 hours
  4. temperatureto cool
  5. filtrationfor filtering insoluble matter out
  6. extractionAn organic layer was extracted from a mother liquor
  7. washwashed with water
  8. dry with materiala saturated sodium chloride solution, and dried with anhydrous sodium sulfate
  9. distillationthe solvent was distilled off under reduced pressure
  10. customThe residue was purified by means of silica gel column chromatography