反应详情

7.8 g (26 mmol) of 4′-bromo-N-methyl-2′-amino-benzanilide were suspended into 50 mL of xylene. Then, 1.5 g (7.7 mmol) of p-toluenesulfonic acid monohydrate was added, and the whole was refluxed under heating for 7 hours. After the completion of the reaction, the resultant was filtered. The resultant solid was dissolved into methylene chloride, washed with 10-mass % K2CO3 and a saturated sodium chloride solution, and dried with magnesium sulfate. After that, the solvent was distilled off under reduced pressure. The filtrate was washed with 10-mass % K2CO3 and a saturated sodium chloride solution, and dried with magnesium sulfate. After that, the solvent was distilled off under reduced pressure. The resultant two residues were coalesced, and the resultant was purified by means of silica gel column chromatography to obtain 6.5 g of 5-bromo-1-methyl-2-phenyl-1H-benzimidazole as a white solid (89% yield).

1. temperaturethe whole was refluxed
2. temperatureunder heating for 7 hours
3. customAfter the completion of the reaction
4. filtrationthe resultant was filtered
5. dissolutionThe resultant solid was dissolved into methylene chloride
6. washwashed with 10-mass % K2CO3
7. dry with materiala saturated sodium chloride solution, and dried with magnesium sulfate
8. distillationAfter that, the solvent was distilled off under reduced pressure
9. washThe filtrate was washed with 10-mass % K2CO3
10. dry with materiala saturated sodium chloride solution, and dried with magnesium sulfate
11. distillationAfter that, the solvent was distilled off under reduced pressure
12. customthe resultant was purified by means of silica gel column chromatography