反应详情

Sodium methoxide (94 mg, 1.74 mmol) was added to a solution of 2-bromo-6-methyl-4-nitro-pyridine 1-oxide (408 mg, 1.74 mmol) in dry methanol (20 mL) at 0° C., then warmed to ambient temperature and maintained overnight. The volatiles were evaporated in vacuo and the residue extracted with chloroform (5×40 mL). The combined organic layers were washed with water, dried over anhydrous sodium sulfate and concentrated to afford a residue which was purified by column chromatography over silica gel (60-120 mesh) using 3% methanol in chloroform as eluent to afford 2-bromo-4-methoxy-6-methyl-pyridine 1-oxide (0.32 g, 84%) as a white solid.

1. temperaturemaintained overnight
2. customThe volatiles were evaporated in vacuo
3. extractionthe residue extracted with chloroform (5×40 mL)
4. washThe combined organic layers were washed with water
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated
7. customto afford a residue which
8. customwas purified by column chromatography over silica gel (60-120 mesh)