反应详情

温度

100 °C

To a solution of ethyl 4-formyl-pyrazole-3-carboxylate (1.70 g, 10.1 mmol) and 3-chloro-2-fluoropyridine (1.99 g, 15.1 mmol) in dimethylformamide (20 mL) is added potassium carbonate (2.80 g, 20.2 mmol) and the mixture is stirred at 100° C. for 16 hours. After completion, the reaction mixture is partitioned between water (25 mL) and ethyl acetate (25 mL). The aqueous layer is extracted with ethyl acetate (3×25 mL) and the combined organic extracts are dried over sodium sulfate, concentrated in vacuo and purified by column chromatography over silica gel eluting with hexane/ethyl acetate (50:50) to yield 1.5 g (54%) of the title compound. MS (m/z): 280 (M+1).

1. customAfter completion, the reaction mixture is partitioned between water (25 mL) and ethyl acetate (25 mL)
2. extractionThe aqueous layer is extracted with ethyl acetate (3×25 mL)
3. dry with materialthe combined organic extracts are dried over sodium sulfate
4. concentrationconcentrated in vacuo
5. custompurified by column chromatography over silica gel eluting with hexane/ethyl acetate (50:50)