反应详情

温度

100 °C

To a solution of 3-hydoxypyridine sodium salt (purchased from Acros) (2.54 g, 26.71 mmol) in N,N-dimethyl formamide (50 mL) was added 2-fluoronicotinonitrile (3.32 g, 26.68 mmol) dropwise and the solution was heated at 100° C. for 2 hours. To the reaction mixture was added ethyl acetate (100 mL) and 1M NaHCO3 (150 mL) and it was filtered to remove black tar. The filtrate was decolorized with activated charcoal and extracted with ethyl acetate (3×30 ml). The combined organic extracts were dried (Na2SO4), filtered and concentrated. The crude product was purified by flash column chromatography on silica gel using dichloromethane to give the title compound. MS (ESI+) m/z 197 (M+H)+.

1. filtrationwas filtered
2. customto remove black tar
3. extractionextracted with ethyl acetate (3×30 ml)
4. dry with materialThe combined organic extracts were dried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customThe crude product was purified by flash column chromatography on silica gel