反应详情

Sodium hydride (1.26 g, 52.75 mmol, 60% oil dispersion) was washed with petroleum ether under a nitrogen atmosphere. The supernatant was removed after the solids settled. Then a solution of 2-(4-fluoro-1H-pyrazol-1-yl)acetonitrile (1.1 g, 8.79 mmol) and 1,2-dibromoethane (2.28 mL, 26.37 mmol) in dimethylsulfoxide (90 mL) was added at 0° C. over a period of 40 min. The reaction mixture was stirred at room temperature for 6 h. A saturated aqueous solution of ammonium chloride was added and the mixture was extracted with diethyl ether. The organic layer was washed with brine, dried over sodium sulfate, filtered and concentrated under reduced pressure. The crude material was purified via column chromatography (100-200 mesh silica gel, 5-12% ethyl acetate in petroleum ether) to afford 1-(4-fluoro-1H-pyrazol-1-yl)cyclopropanecarbonitrile (300 mg).

1. customThe supernatant was removed after the solids
2. extractionthe mixture was extracted with diethyl ether
3. washThe organic layer was washed with brine
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe crude material was purified via column chromatography (100-200 mesh silica gel, 5-12% ethyl acetate in petroleum ether)