反应详情

To a stirred solution of 1-(5-bromopyridin-3-yl)ethanone (5.0 g, 25.0 mmol) in anhydrous MeOH (50 mL) at 0° C., was added NaBH4 (1.32 g, 35.0 mmol) and the reaction was allowed to warm to room temperature. All solvent was removed. The residue was dissolved in cold water and extracted with EtOAc (2×70 mL). The combined organic layers was dried with Na2SO4 and concentrated under reduced pressure. The residue was purified by column chromatography (40% EtOAc in hexanes) to provide 4.555 g of 1-(5-bromopyridin-3-yl)ethanol.

1. customAll solvent was removed
2. dissolutionThe residue was dissolved in cold water
3. extractionextracted with EtOAc (2×70 mL)
4. dry with materialThe combined organic layers was dried with Na2SO4
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by column chromatography (40% EtOAc in hexanes)