反应详情

温度

5 °C

POBr3 (222.8 g, 0.78 mol) was added in portions to 2-hydroxy-5-methyl-3-nitropyridine (100 g, 0.65 mol) in DMF (500 mL) with stirring at 0-10° C. then the reaction mixture was stirred at 80° C. under nitrogen for 12 hours. Reaction mixture was cooled and poured into crushed ice (1 Kg), obtained solid was filtered, washed thoroughly with ice-cold water (2×500 mL), dried in a desiccator under high vacuum for one day to obtain 2-bromo-5-methyl-3-nitropyridine as yellow solid (121 g) in 86% yield. (M+H) Expected: 217; found 216.9.

1. stirringthe reaction mixture was stirred at 80° C. under nitrogen for 12 hours
2. customReaction mixture
3. temperaturewas cooled
4. additionpoured
5. customobtained solid
6. filtrationwas filtered
7. washwashed thoroughly with ice-cold water (2×500 mL)
8. customdried in a desiccator under high vacuum for one day