反应详情

温度

100 °C

A solution of 21 g (0.071 mol) of 2-(4-chlorophenyl)-2-[1-(3-chloro-1,2,4-triazol-1-yl)-cyclopropyl]-oxirane in 30 ml of absolute dimethylformamide is added dropwise at 80° C. to a stirred mixture of 15.6 g (0.276 mol) of 1,2,4-triazole and 1.7 g (0.015 mol) of potassium tert.-butylate in 40 ml of absolute dimethylformamide. The reaction mixture is stirred for 6 more hours at 100° C. and then concentrated by stripping off the solvent under reduced pressure. The residue which remains is taken up in a mixture of ethyl acetate/toluene, and the mixture is washed with water, dried over sodium sulphate and concentrated under reduced pressure. The residue is chromatographed on silica gel using a mixture of dichloromethane/ethanol=98:2 as the eluent. Concentration of the eluate by evaporation gives 11.5 g of 1-(4-chlorophenyl)-1-[1-(3-chloro-1,2,4-triazol-1-yl)-cyclopropyl]-2-(1,2,4-triazol-1-yl)-ethan-1-ol in the form of a solid of melting point 156° C.

1. concentrationconcentrated
2. additionThe residue which remains is taken up in a mixture of ethyl acetate/toluene
3. washthe mixture is washed with water
4. dry with materialdried over sodium sulphate
5. concentrationconcentrated under reduced pressure
6. customThe residue is chromatographed on silica gel using
7. additiona mixture of dichloromethane/ethanol=98:2 as the eluent
8. customConcentration of the eluate by evaporation