反应详情

Suspending 7.8 g (26 mmol) of 4′-bromo-N-methyl-2′-amino-benzanilide obtained in the above step (3) into 50 milliliter of xylene, and adding 1.5 g (7.7 mmol) of p-toluenesulfonic acid 1 hydrate, the resultant solution was refluxed with heating for 7 hours. After completing the reaction, the resultant solution was filtered. Dissolving the resultant solids into methylene chloride, the resultant solution was washed with 10% K2CO3 aqueous solution and with a saturated solution of sodium chloride, and then, after drying with the use of magnesium sulfate, the solvent was removed by distillation. Washing the filtrate with 10% K2CO3 aqueous solution and with saturated solution of sodium chloride, and then, after drying with the use of magnesium sulfate, the solvent was removed by distillation. Combining the above two kinds of residues after removing by distillation, the resultant product was refined with silicagel column chromatography, 6.50 g of 5-bromo-1-methyl-2-phenyl-1H-benzimidazole was obtained as white solids (yield: 89%).

1. temperaturewith heating for 7 hours
2. customthe reaction
3. filtrationthe resultant solution was filtered
4. dissolutionDissolving the resultant solids into methylene chloride
5. washthe resultant solution was washed with 10% K2CO3 aqueous solution and with a saturated solution of sodium chloride
6. dry with materialafter drying with the use of magnesium sulfate
7. customthe solvent was removed by distillation
8. washWashing the filtrate with 10% K2CO3 aqueous solution
9. dry with materialwith saturated solution of sodium chloride, and then, after drying with the use of magnesium sulfate
10. customthe solvent was removed by distillation
11. customafter removing by distillation