反应详情

Sodium bicarbonate (1.70 g, 16.89 mmol) and benzyl chloroformate (1.58 g, 9.29 mmol) were added to a solution of 3-aminopyridin-2(1H)-one (0.930 g, 8.45 mmol) in tetrahydrofuran (20 mL). After 7 h, the mixture was extracted with ethyl acetate and saturated sodium bicarbonate. The organic extract was washed with water and saturated brine, dried over magnesium sulfate, filtered, and concentrated. Purification by chromatography [silica gel, 1% to 5% methanol (10% ammonium hydroxide) in dichloromethane gradient elution] gave the title compound (1.304 g). MS 245 (M+1)

1. extractionthe mixture was extracted with ethyl acetate and saturated sodium bicarbonate
2. extractionThe organic extract
3. washwas washed with water and saturated brine
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customPurification
8. washby chromatography [silica gel, 1% to 5% methanol (10% ammonium hydroxide) in dichloromethane gradient elution]