反应详情

7.24 g of crude 4-[1-hydroxycyclohex-1-yl-1-(1,2,4-triazolyl)methyl]benzonitrile is dissolved at 0° in 50 ml of dichloromethane and stirred for 1 hour at 0° with 22.7 ml of thionyl chloride. Then the mixture is concentrated to dryness under vacuum, dissolved in 50 ml of dichloromethane, stirred with 30 ml of triethylamine for 2 hours, diluted with water, extracted four times with ethyl acetate, washed with sodium chloride solution, dried over sodium sulfate, concentrated to dryness under vacuum, and chromatographed on silica gel with hexane/ethyl acetate, yielding 1.45 g of 4-[1-cyclohexylidene-1-(1,2,4-triazolyl)methyl]benzonitrile as a free base, mp 92-93°.

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