反应详情

温度

60 °C

A solution of 4.2 g of methyl 2-fluorophenylglyoxalate in 30 ml of anhydrous dimethyl sulfoxide was added dropwise to a solution of 5.0 g of the potassium salt of 1-(4-chlorophenyl)-3-hydroxy-pyrazole in 30 ml of anhydrous dimethyl sulfoxide. The batch was heated at 60° C. for 3.5 more hours, cooled and divided into two halves. One half was poured into ice-water/methyl tert-butyl ether for working-up. After the organic phase had been separated off, the aqueous phase was extracted three more times with methyl tert-butyl ether. The combined organic phases were dried over sodium sulfate and concentrated. The crude product was purified by chromatography over silica gel (eluent heptane/ethyl acetate 80/20→70/30). This gave 1.0 g of the title compound as a pale oil.

1. temperaturecooled
2. customAfter the organic phase had been separated off
3. extractionthe aqueous phase was extracted three more times with methyl tert-butyl ether
4. dry with materialThe combined organic phases were dried over sodium sulfate
5. concentrationconcentrated
6. customThe crude product was purified by chromatography over silica gel (eluent heptane/ethyl acetate 80/20→70/30)