反应详情

5-(methylthio)-2-nitropyridine (270 g), iron powder (600 g), acetic acid (500 mL) and water (2 L) were heated to reflux for 4 hours. Then saturated sodium bicarbonate solution (6 L) was added into the reaction mixture. The reaction mixture was filtered, and the filtrate was extracted with ethyl acetate. The organic phase was washed with saturated NaCl solution, and dried with anhydrous sodium sulfate. After filtration, the residual solution was removed under reduced pressure to obtain the target compound (185 g). 1H-NMR (300 MHz, CDCl3): δ 2.39 (3H, s), 4.49 (2H, brs), 6.47 (1H, d), 7.50 (1H, dd), 8.11 (1H, d). LC-MS m/z: 141 [M++1].

1. temperatureto reflux for 4 hours
2. filtrationThe reaction mixture was filtered
3. extractionthe filtrate was extracted with ethyl acetate
4. washThe organic phase was washed with saturated NaCl solution
5. dry with materialdried with anhydrous sodium sulfate
6. filtrationAfter filtration
7. customthe residual solution was removed under reduced pressure