反应详情

温度

70 °C

Concentrated nitric acid (4 mL) was added to cold concentrated sulfuric acid (7 mL). 2-Bromo-6-methyl-pyridine 1-oxide (820 mg, 4.36 mmol) was added to this and then heated at 70° C. for 4 h. The mixture was cooled and poured slowly into ice-cold water (100 mL) and basified to pH ˜8 with sodium bicarbonate solution. This was extracted with ethyl acetate (4×50 mL) then the combined organic layers were dried over anhydrous sodium sulfate and concentrated to give a residue which was purified by washing with pentane (50 mL) to afford 2-bromo-6-methyl-4-nitro-pyridine 1-oxide (0.41 g, 40%) as a free flowing yellow solid.

1. temperatureThe mixture was cooled
2. extractionThis was extracted with ethyl acetate (4×50 mL)
3. dry with materialthe combined organic layers were dried over anhydrous sodium sulfate
4. concentrationconcentrated
5. customto give a residue which
6. customwas purified
7. washby washing with pentane (50 mL)