反应详情

温度

110 °C

POCl3 (20.0 mL) was added to 6-nitrothieno[3,2-b]pyridin-7-ol (1.56 g, 7.95 mmol). The mixture was stirred at 110° C. for 3 h. The reaction mixture was then concentrated under reduced pressure. The resulting residue was dissolved in DCM (150 mL), and a saturated aq. NaHCO3 (150 mL) was added slowly. The organic layer was washed with water (100 mL) and brine (100 mL), then dried over Na2SO4 and concentrated under reduced pressure. The residue was purified by chromatography on silica gel (0 to 30% EtOAc in hexanes) to afford the sub-title compound as a pale yellow solid (1.39 g, 82%). LCMS calc. for C2H4ClN2O2S (M+H)+: m/z=215.0. found 215.0.

1. concentrationThe reaction mixture was then concentrated under reduced pressure
2. dissolutionThe resulting residue was dissolved in DCM (150 mL)
3. additiona saturated aq. NaHCO3 (150 mL) was added slowly
4. washThe organic layer was washed with water (100 mL) and brine (100 mL)
5. dry with materialdried over Na2SO4
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by chromatography on silica gel (0 to 30% EtOAc in hexanes)