反应详情

7.1 g of crude 4-[1-hydroxycyclopent-1-yl-1-(1,2,3-triazolyl)methyl]benzonitrile is dissolved at 0° in 50 ml of dichloromethane and stirred with 24 ml of thionyl chloride for 1 hour at 0°. Then the mixture is concentrated to dryness under vacuum, dissolved in 50 ml of dichloromethane, stirred with 32 ml of triethylamine for 2 hours, diluted with water, extracted three times with ethyl acetate, washed with water, dried over sodium sulfate, concentrated to dryness under vacuum, and chromatographed on silica gel with hexane/ethyl acetate, yielding 2.1 g of 4-[1-cyclopentylidene-1-(1,2,3-triazolyl)methyl]benzonitrile as the free base, 108°-109° C.

1. concentrationThen the mixture is concentrated to dryness under vacuum
2. dissolutiondissolved in 50 ml of dichloromethane
3. additiondiluted with water
4. extractionextracted three times with ethyl acetate
5. washwashed with water
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated to dryness under vacuum
8. customchromatographed on silica gel with hexane/ethyl acetate