反应详情

温度

0 °C

To a solution of 3-(3-nitropyridin-4-yl)cyclohex-2-en-1-ol (1.0 g, 4.5 mmol), phthalimide (1.0 g, 6.8 mmol) and triphenylphosphine (1.8 g, 6.8 mmol) in THF (20 mL), di-tert-butyl azodicarboxylate (1.6 g, 6.8 mmol) was added slowly at 0° C. The resulting mixture was stirred at 0° C. for 3 h. After concentrated concentrating under reduced pressure, the crude product was purified by silica gel column chromatography (eluting with 0-70% EtOAc in hexanes) to give a solid, which was further treated with DCM and hexanes to yield sub-title compound (1.55 g, 98%). LCMS calc. for C19H16N3O4 (M+H)+: m/z=350.1. Found: 350.3.

1. concentrationAfter concentrated
2. concentrationconcentrating under reduced pressure
3. customthe crude product was purified by silica gel column chromatography (eluting with 0-70% EtOAc in hexanes)
4. customto give a solid, which