反应详情

A suspension of 831 mg (5 mmol) of 3-cyano-4-fluoronitrobenzene, of 0.82 g (10 mmol) 4-methylimidazol and of 1.38 g (10 mmol) potassium carbonate in acetonitrile (10 mL) was stirred for 60 h at 20° C. The solvent was evaporated and the residue was partitioned between ethyl acetate and 1N aqueous sodium hydroxide solution. The aqueous layer was extracted with ethyl acetate. The combined organic layers were washed with brine, dried over sodium sulphate, and the solvent was evaporated under reduced pressure. The crude product was crystallized from ethanol/water yielding the title compound (0.65 g, 57%) as an off-white solid. 1H NMR (DMSO-D6, 250 MHz): δ (ppm)=8.95 (s, 1H), 8.62 (d, 1H), 8.16 (s, 1H), 7.93 (d, 1H), 7.49 (s, 1H), 2.21 (s, 3H).

1. customThe solvent was evaporated
2. customthe residue was partitioned between ethyl acetate and 1N aqueous sodium hydroxide solution
3. extractionThe aqueous layer was extracted with ethyl acetate
4. washThe combined organic layers were washed with brine
5. dry with materialdried over sodium sulphate
6. customthe solvent was evaporated under reduced pressure
7. customThe crude product was crystallized from ethanol/water yielding the title compound (0.65 g, 57%) as an off-white solid