反应详情

温度

80 °C

To a suspension of 2-bromo-3-methyl-5-nitropyridine (10.01 g), isopropanol (130 ml), water (26 ml) and iron (12.9 g) was added acetic acid (5.27 ml), and stirred at 80° C. for 3.5 hours. To the reaction solution was added potassium carbonate (13.37 g), filtered through Celite, then extracted with ethyl acetate, washed with saturated brine, dried over anhydrous sodium sulfate, and the solvent was evaporated in vacuo. The precipitated solid was collected by filtration to give 5-amino-2-bromo-3-methylpyridine (6.66 g) as a gray solid. MS (ESI) m/z: 187, 189 (M+H)+.

1. filtrationfiltered through Celite
2. extractionextracted with ethyl acetate
3. washwashed with saturated brine
4. dry with materialdried over anhydrous sodium sulfate
5. customthe solvent was evaporated in vacuo
6. filtrationThe precipitated solid was collected by filtration