反应详情

2.1 g (5.7 mmol) of N-[2-(4-bromophenylamino)phenyl]benzamide was suspended in 30 mL of xylene. To the resulting suspension, 0.6 g (2.9 mmol) of p-toluenesulfonic acid monohydrate was added, and the resultant was subjected to azeotropic dehydration while heating under reflux for 3 hours. After allowing it to be cool, ethyl acetate, methylene chloride and water were added to the reaction solution, and unsoluble matters were filtered off. An organic phase was extracted from a mother solution, washed with water and saturated saline, and dried with anhydrous sodium sulfate. The solvent was distilled off under a reduced pressure. Residues were purified by silica gel column chromatography, whereby 1.0 g of slightly pinky white crystals of 1-(4-bromophenyl)-2-phenyl-1H-benzimidazole were obtained (yield 52%).

1. temperaturewhile heating
2. temperatureunder reflux for 3 hours
3. temperatureto be cool
4. filtrationwere filtered off
5. extractionAn organic phase was extracted from a mother solution
6. washwashed with water and saturated saline
7. dry with materialdried with anhydrous sodium sulfate
8. distillationThe solvent was distilled off under a reduced pressure
9. customResidues were purified by silica gel column chromatography, whereby 1.0 g of slightly pinky white crystals of 1-(4-bromophenyl)-2-phenyl-1H-benzimidazole
10. customwere obtained (yield 52%)