反应详情

4-hydroxy-2-methylbenzimidazole (0.59 g, 4 mmol) was dissolved in acetonitrile (15 ml). To the solution were added 2,6-dimethylbenzylchloride (0.52 g, 4 mmol) and sodium hydroxide (0.16 g, 4 mmol) (dissolved in 1 ml water) and the reaction mixture was refluxed for 2 h. The solvent was evaporated under reduced pressure and the residue was dissolved in methylene chloride and was washed with 2 M NaOH. The organic layer was separated, dried over sodium sulfate and evaporated under reduced pressure. The oily residue was purified by column chromatography on silica gel. The product was eluted with methylene chloride containing 5% methanol. Crystallization from acetonitrile gave 0.18 g (18%) of the title compound.

1. temperaturethe reaction mixture was refluxed for 2 h
2. customThe solvent was evaporated under reduced pressure
3. dissolutionthe residue was dissolved in methylene chloride
4. washwas washed with 2 M NaOH
5. customThe organic layer was separated
6. dry with materialdried over sodium sulfate
7. customevaporated under reduced pressure
8. customThe oily residue was purified by column chromatography on silica gel
9. washThe product was eluted with methylene chloride containing 5% methanol
10. customCrystallization from acetonitrile