反应详情

In 45 ml of ethanol was dissolved 9.10 g (20.1 mmol) of 5-(3,5-dichlorophenylthio)-1-methyl-4-isopropyl-2-(p-methoxybenzyloxymethyl)-1H-imidazole (17b), followed by addition of 90 ml of 6N-hydrochloric acid, and the mixture was refluxed for 1 hour. This reaction mixture was concentrated under reduced pressure to remove ethanol and the residue forming a couple of layers was extracted twice with n-hexane to remove p-methoxybenzyl chloride. The aqueous layer was extracted with methylene chloride and the extract was neutralized with an aqueous sodium bicarbonate solution and dried over magnisium sulfate. The solvent was then distilled off under reduced pressure and the residue was rinsed with isopropyl ether to provide 6.3 g (yield 95%) of [5-(3,5-dichlorophenylthio)-4-isopropyl-1-methyl-1H-imidazol-2-yl]methanol (12=Compound I-8). mp 157-158° C.

1. temperaturethe mixture was refluxed for 1 hour
2. concentrationThis reaction mixture was concentrated under reduced pressure
3. customto remove ethanol
4. customthe residue forming a couple of layers
5. extractionwas extracted twice with n-hexane
6. customto remove p-methoxybenzyl chloride
7. extractionThe aqueous layer was extracted with methylene chloride
8. dry with materialdried over magnisium sulfate
9. distillationThe solvent was then distilled off under reduced pressure
10. washthe residue was rinsed with isopropyl ether