反应详情

温度

60 °C

To a solution of 1-(3-pyridyl)-1-butanone (20.0 g) in 47% aqueous hydrobromic acid (40 ml) and acetic acid (40 ml) was added bromine (15.2 ml), and the mixture was stirred at 60° C. for 30 minutes. The reaction mixture was poured into ice-water, and after adding a saturated aqueous sodium thiosulfate solution, potassium carbonate was added to the mixture to adjust pH to 4. The reaction mixture was extracted with ethyl acetate, washed successively with a saturated aqueous sodium hydrogen carbonate solution and brine, and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure to obtain a crude product of 2-bromo-1-(3-pyridyl)-1-butanone (30.15 g) as brownish oil.

1. additionwas added to the mixture
2. extractionThe reaction mixture was extracted with ethyl acetate
3. washwashed successively with a saturated aqueous sodium hydrogen carbonate solution and brine
4. dry with materialdried over anhydrous sodium sulfate
5. customThe solvent was removed under reduced pressure