反应详情

To a suspension of 3-nitropyridin-4-ol (4.342 g, 31 mmol) in toluene (60 mL) was added POCl3 (11.6 mL, 124.4 mmol) at 0° C. The resulting mixture was warmed to room temperature, then heated to 110° C. for 14 hours. After cooling to room temperature, the solvent was removed in vacuo and the residue was poured into ice, and basified with saturated aqueous NH4Cl solution. The mixture was extracted with EtOAc (40 mL×2). The combined organic layers was washed with water, brine, dried (MgSO4) and concentrated to a brown oil, which solidified on standing. (3.68 g, 75% yield).

1. temperatureheated to 110° C. for 14 hours
2. temperatureAfter cooling to room temperature
3. customthe solvent was removed in vacuo
4. additionthe residue was poured into ice
5. extractionThe mixture was extracted with EtOAc (40 mL×2)
6. washThe combined organic layers was washed with water, brine
7. dry with materialdried (MgSO4)
8. concentrationconcentrated to a brown oil, which