反应详情

To a solution of N-(2-azidopyridin-4-yl)-2,4,6-trichlorobenzamide (90 mg, 0.26 mmol) in ethanol (5 mL) was added SnCl2.2H2O (300 mg, 1.31 mmol). The mixture was heated at reflux for 1 hour and then cooled to room temperature. The reaction was concentrated under reduced pressure and the residue was diluted with water (10 mL). The mixture was extracted with ethyl acetate (3×5 mL). The combined organic extracts were dried over MgSO4 and concentrated under reduced pressure to give N-(2-aminopyridin-4-yl)-2,4,6-trichlorobenzamide (82 mg, yield: 100%). LCMS (ESI) m/z: 316.0 [M+H+].

1. temperatureThe mixture was heated
2. temperatureat reflux for 1 hour
3. concentrationThe reaction was concentrated under reduced pressure
4. additionthe residue was diluted with water (10 mL)
5. extractionThe mixture was extracted with ethyl acetate (3×5 mL)
6. dry with materialThe combined organic extracts were dried over MgSO4
7. concentrationconcentrated under reduced pressure