反应详情

6.9 g of crude 4-[1-hydroxycyclopent-1-yl-1-(imidazolyl)methyl]benzonitrile is refluxed in 82 ml of thionyl chloride to 0.5 hour. Then the mixture is concentrated to dryness under vacuum, combined with 2 N sodium hydroxide solution, extracted with dichloromethane, dried over sodium sulfate, concentrated to dryness under vacuum, and chromatographed on silica gel with hexane/ethyl acetate, thus producing 3.1 g of 4-[1-cyclopentylidene-1-(imidazolyl)methyl]benzonitrile as the free base, mp 108°-110°.

1. concentrationThen the mixture is concentrated to dryness under vacuum
2. extractionextracted with dichloromethane
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated to dryness under vacuum
5. customchromatographed on silica gel with hexane/ethyl acetate