反应详情

100 g (0.66 mol) of 1-chloro-cyclopropyl chloromethyl ketone in 80 ml of acetonitrile are added dropwise to a refluxing suspension of 83 g (0.6 mol) of potassium carbonate and 58 g (0.84 mol) of triazole in 330 ml of acetonitrile. The mixture is refluxed for 8 hours and then filtered off with suction and concentrated. The residue is taken up in ethyl acetate/toluene, and the mixture is washed with water, dried over sodium sulphate and concentrated. The subsequent purification by column chromatography in which dichloromethane was used as the mobile phase gave 62 g (51% of theory) of 1-(1-chlorocyclopropyl)-2-(1,2,4-triazol-1-yl)-ethan-1-one.

1. temperatureThe mixture is refluxed for 8 hours
2. filtrationfiltered off with suction
3. concentrationconcentrated
4. washthe mixture is washed with water
5. dry with materialdried over sodium sulphate
6. concentrationconcentrated
7. customThe subsequent purification by column chromatography in which dichloromethane