反应详情

2-Bromo-6-methyl-4-nitro-pyridine 1-oxide (4 g, 17 mmol) was dissolved in methanol (anhydrous, 100 ml), and sodium methoxide (1.8 g, 33 mmol) was added. The mixture was stirred at room temperature for 90 minutes, diluted with water (90 ml) and concentrated under reduced pressure to half of its volume. The mixture was extracted with DCM (5×), the combined organic phases were dried (sodium sulfate) and concentrated to dryness under reduced pressure to yield 3.3 g of yellow crystals, 15 mmol, 88%) MS(APCI) m/z=217.9 [M+1]+.

1. concentrationconcentrated under reduced pressure to half of its volume
2. extractionThe mixture was extracted with DCM (5×)
3. dry with materialthe combined organic phases were dried (sodium sulfate)
4. concentrationconcentrated to dryness under reduced pressure