反应详情

温度

85 °C

2-Bromo-3-fluoro-6-methylpyridine (3.60 g, 18.9 mmol) was dissolved in 10 mL of pyridine in pressure tube. To this was added 50 mL of water, and the mixture was warmed to 85° C. Potassium permanganate (5.99 g, 37.9 mmol) was added, the tube was capped, and the mixture was stirred at 85° C. for 48 hours. The mixture was filtered through GF/F filter paper, and the filtrate was concentrated to about half volume under reduced pressure. The remaining material was acidified to pH 4 with 1M aqueous HCl and extracted with EtOAc. The combined organic extracts were dried over sodium sulfate and concentrated under reduced pressure to give 0.70 g of the title compound (17%).

1. customthe tube was capped
2. filtrationThe mixture was filtered through GF/F
3. filtrationfilter paper
4. concentrationthe filtrate was concentrated to about half volume under reduced pressure
5. extractionextracted with EtOAc
6. dry with materialThe combined organic extracts were dried over sodium sulfate
7. concentrationconcentrated under reduced pressure