反应详情

In 20 ml of acetone was dissolved 5.0 g of the imidazole (101a) and 1.36 g (14.7 mmol) of monochloroacetone, followed by addition of 2.46 g (12.27 mmol) of potassium iodide, and the mixture was stirred at room temperature for 30 minutes. Then, to the mixture was added 2.04 g (14.8 mmol) of potassium carbonate, and the mixture was stirred with heating at 50° C. for 4 hours and worked up. The reaction mixture was distilled off under reduced pressure, and the residue was extracted with methylene chloride. The extract was washed with water, dried and the solvent was distilled off. The residue was purified by silica gel column chromatography (methylene chloride:ethyl acetate=9:1) to provide 3.1 g (yield 54%) of 2-benzyloxymethyl-5-(3,5-dichlorophenylthio)-4-isopropyl-1-acetylmethyl-1H-imidazole (139) as solid.

1. stirringthe mixture was stirred
2. temperaturewith heating at 50° C. for 4 hours
3. distillationThe reaction mixture was distilled off under reduced pressure
4. extractionthe residue was extracted with methylene chloride
5. washThe extract was washed with water
6. customdried
7. distillationthe solvent was distilled off
8. customThe residue was purified by silica gel column chromatography (methylene chloride:ethyl acetate=9:1)