反应详情

温度

100 °C

A mixture of 6-hydroxy-2,4-dimethyl-5-nitronicotinonitrile (step 2, 3.2 g, 16.6 mmol) and phosphorus oxychloride (20 mL) was stirred at 100° C. for 16 h. After cooling, the mixture was poured in water (100 mL). The resulting mixture was extracted with dichloromethane (3×100 mL). The organic layer was washed with brine (50 mL), dried (MgSO4), and concentrated to afford 2.3 g (66%) of the title compound as brown solids: 1H-NMR (DMSO-d6) δ 2.82 (3H, s), 2.52 (3H, s).

1. temperatureAfter cooling
2. extractionThe resulting mixture was extracted with dichloromethane (3×100 mL)
3. washThe organic layer was washed with brine (50 mL)
4. dry with materialdried (MgSO4)
5. concentrationconcentrated