反应详情

温度

70 °C

A mixture of 3-fluoro-4-methylpyridine-2-carbonitrile (2.1 g, 15.43 mmol), 3-bromo-5-chlorophenol (3.68 g, 17.74 mmol) and cesium carbonate (5.03 g, 15.43 mmol) in DMF (30 mL) was heated at 70° C. for 1 hour and then at 80° C. for another hour, after which the mixture was partitioned between water (300 mL) and ethyl acetate (2×500 mL). The combined extracts were washed with water (100 mL) and then brine (100 mL), dried over MgSO4, filtered, and the solvent removed in vacuo. The residue was chromatographed using RediSep column (330 g) and eluted with a gradient of 0-10% EtOAc/CH2Cl2 and the pure fractions combined and concentrated on the rotary evaporator to give the title compound. LRMS (M+1)=324.9.

1. waitat 80° C. for another hour
2. customafter which the mixture was partitioned between water (300 mL) and ethyl acetate (2×500 mL)
3. washThe combined extracts were washed with water (100 mL)
4. dry with materialbrine (100 mL), dried over MgSO4
5. filtrationfiltered
6. customthe solvent removed in vacuo
7. customThe residue was chromatographed
8. washeluted with a gradient of 0-10% EtOAc/CH2Cl2
9. concentrationconcentrated on the rotary evaporator