反应详情

温度

110 °C

A mixture of 2,6-dichloro-3-methylpyridine (2.20 g, 13.6 mmol) in concentrated sulfuric acid (11.3 mL) was treated with fuming nitric acid (6.65 mL) and heated to 110° C. for 3 hours. The reaction mixture was poured into ice-water and neutralized with 2N sodium hydroxide. The mixture was extracted with dichloromethane (3×70 mL) and the combined extracts were dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to yield 2,6-dichloro-3-methyl-5-nitropyridine (2.43 g, 86%). 400 M Hz 1H NMR (DMSO-d6) δ: 8.66 (s, 1H), 2.39 (s, 3H).

1. extractionThe mixture was extracted with dichloromethane (3×70 mL)
2. dry with materialthe combined extracts were dried over anhydrous sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure