反应详情

In the course of 3 hours, 60 g (2 mols of sodium hydride (80% strength in paraffin oil) are added to a solution of 138 g (2 mols of 1,2,4-triazole in 1,600 ml of absolute dimethylformamide, with vigorous evolution hydrogen. The mixture is stirred for a further 30 minutes at room temperature. 388 g (2 mols of 3,3-dimethyl -4-[(methylsulphonyl)oxy]-2-butanone are then added dropwise in the course of 15 minutes. The reaction mixture is then stirred for 16 hours at 95° C. 100 ml of water are firstly added carefully to the reaction mixture, and the mixture is then poured into 4 1 of water. The mixture is extracted six times with dichloromethane. The combined organic phases are washed once with plenty of water, dried over sodium sulphate and concentrated under a high vacuum. After column chromatography (silica gel; dichloromethane/ethyl acetate=1:1), 290 g (86.8% of 3,3-dimethyl -4-(1,2,4-triazol-1-yl)-2-butanone are obtained as an oil with a content of 97% after GC.

1. stirringThe reaction mixture is then stirred for 16 hours at 95° C
2. extractionThe mixture is extracted six times with dichloromethane
3. washThe combined organic phases are washed once with plenty of water
4. dry with materialdried over sodium sulphate
5. concentrationconcentrated under a high vacuum