反应详情

温度

100 °C

To a solution of 2-amino-5-bromo-nicotinic acid (1.0 g, 4.60 mmol) in POCl3 (20 mL) was added isobutyric acid hydrazide (705 mg, 6.912 mmol) at RT. The reaction temperature was slowly heated to 100° C. and stirred for 18 h. The solvent was evaporated under reduced pressure, the residue was basified with saturated cold sodium bicarbonate solution (50 mL), extracted with ethyl acetate (3×50 mL), organic layer was washed with brine, dried over anhydrous sodium sulphate and concentrated under reduced pressure. Crude compound was purified by column chromatography using 100-200 mesh silica gel. The column was eluted with 40% EtOAc in petroleum ether to afford the title compound as a yellow solid.

1. customThe solvent was evaporated under reduced pressure
2. extractionextracted with ethyl acetate (3×50 mL), organic layer
3. washwas washed with brine
4. dry with materialdried over anhydrous sodium sulphate
5. concentrationconcentrated under reduced pressure
6. customCrude compound was purified by column chromatography
7. washThe column was eluted with 40% EtOAc in petroleum ether