反应详情

A flask was charged with sodium hydride (3.99 g, 158 mmol) and DMF (50 mL), and 3-hydroxyisonicotinonitrile (15.8 g, 132 mmol) was added. The reaction was stirred for 2 hours at ambient temperature. 2-Chloro-4-nitropyridine (21.9 g, 138 mmol) was added and the reaction was and stirred overnight. Water was added and the reaction was extracted with ethyl acetate. The organic layer was dried and concentrated. The crude product was purified by silica gel chromatography, eluting with DCM, 5% ammoniated methanol in DCM to give the desired product (0.250 g, 0.820% yield) as yellow solid.

1. additionwas added
2. stirringstirred overnight
3. extractionthe reaction was extracted with ethyl acetate
4. customThe organic layer was dried
5. concentrationconcentrated
6. customThe crude product was purified by silica gel chromatography
7. washeluting with DCM, 5% ammoniated methanol in DCM