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温度

0 °C

In a dry flask, 6-chloro-2-methylpyridin-3-amine (200 mg, 1.40 mmol) and triethylamine (217 μl, 1.56 mmol) were taken up in dichloromethane (7.0 ml) under argon. The solution was cooled to 0° C. and stirred for 20 minutes. Acetic anhydride (134 μl, 1.42 mmol) was added dropwise over 15 minutes. The mixture was allowed to warm to room temperature and left to stir for 22 hours. The reaction was quenched with aqueous sodium bicarbonate and washed with ethyl acetate three times. The organic layers were combined, dried over anhydrous magnesium sulfate, filtered, and concentrated. The resulting crude product was purified by silica gel chromatography (0-100% ethyl acetate/hexanes) to afford the title compound.

1. temperatureto warm to room temperature
2. waitleft
3. stirringto stir for 22 hours
4. customThe reaction was quenched with aqueous sodium bicarbonate
5. washwashed with ethyl acetate three times
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated
9. customThe resulting crude product was purified by silica gel chromatography (0-100% ethyl acetate/hexanes)