反应详情

温度

100 °C

To a mixture of methyl 6-aminopyridine-3-carboxylate (3 g, 19.72 mmol, Aldrich) in 1,4-ioxane (50 mL) was added acetic anhydride (3.72 mL, 39.4 mmol, Aldrich). The resulting mixture was then heated at 85° C. for 3 h and at 100° C. for an additional 3 h. The mixture was then cooled to rt and diluted with EtOAc (400 mL). The mixture was then washed with saturated NaHCO3 solution (2×200 mL), brine (150 mL), dried over MgSO4, and concentrated in vacuo to afford the title compound as a white solid, which was used in the next step without purification. MS (ESI, positive ion) m/z: 195 (M+H).

1. temperatureThe mixture was then cooled to rt
2. washThe mixture was then washed with saturated NaHCO3 solution (2×200 mL), brine (150 mL)
3. dry with materialdried over MgSO4
4. concentrationconcentrated in vacuo