反应详情

With cooling with ice, chloromethyl methyl ether (1.04 mL) and potassium carbonate (3.16 g) were added to an acetone (30 mL) solution of 2-bromo-6-nitropyridin-3-ol (1.0 g), and stirred overnight at room temperature. The reaction liquid was concentrated under reduced pressure, ethyl acetate was added to the residue and washed with water and saturated brine. The organic layer was dried with sodium sulfate, then filtered and concentrated under reduced pressure. The residue was purified through silica gel column chromatography (ethyl acetate/hexane=from 0% to 50%, gradient) to give the intended product (1.16 g, 97%) as a brown solid.

1. customThe reaction liquid
2. concentrationwas concentrated under reduced pressure, ethyl acetate
3. additionwas added to the residue
4. washwashed with water and saturated brine
5. dry with materialThe organic layer was dried with sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe residue was purified through silica gel column chromatography (ethyl acetate/hexane=from 0% to 50%, gradient)