反应详情

温度

10 °C

68 g (0.14 mol) of 4-chloro-3-(4-chloro-5-dibromomethyl-2-fluorophenyl)-5-difluoromethoxy-1-methyl-1H-pyrazole were dissolved in 200 ml of concentrated sulfuric acid, with ice-cooling, whereupon the mixture was heated at 10° C. until the evolution of gas had ceased. It was then poured into 4 l of ice-water. The mixture was subsequently extracted three times using ethyl acetate. The combined organic phases were washed with water, then dried over magnesium sulfate and finally concentrated. The crude product was purified by means of silica gel column chromatography (eluent: hexane/ethyl acetate=8:1). Yield: 35 g; m.p.: 95-98° C.

1. temperaturecooling, whereupon the mixture
2. extractionThe mixture was subsequently extracted three times
3. washThe combined organic phases were washed with water
4. dry with materialdried over magnesium sulfate
5. concentrationfinally concentrated
6. customThe crude product was purified by means of silica gel column chromatography (eluent: hexane/ethyl acetate=8:1)