反应详情

A mixture of 2-bromopyridin-3-ol (3.00 g), ethyl iodide (3.44 ml), anhydrous potassium carbonate (4.28 g) and dry dimethylformamide (34 ml) is stirred under nitrogen at 80°-85° for 2.5 hrs, concentrated to remove solvent, diluted with ethyl acetate (75 ml) and water (40 ml), and the layers are separated. The aqueous phase is extracted with ethyl acetate (75 ml) and the combined organic phase is washed with saline (30 ml), dried over sodium sulfate, and concentrated under reduced pressure to give the title compound, NMR (CDCl3) 7.97, 7.20, 7.12, 4.11 and 1.50δ.

1. concentrationconcentrated
2. customto remove solvent
3. additiondiluted with ethyl acetate (75 ml) and water (40 ml)
4. customthe layers are separated
5. extractionThe aqueous phase is extracted with ethyl acetate (75 ml)
6. washthe combined organic phase is washed with saline (30 ml)
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated under reduced pressure