反应详情

温度

-78 °C

Under cooling at −78° C., 1.56M n-butyllithium in hexane (27 mL) was added dropwise to 2-bromo-5-chloropyridine (6.8 g) in diethyl ether (45 mL), and then N,N-dimethylacetamide (5 mL) was added dropwise thereto, followed by stirring for 30 minutes. The reaction mixture was partitioned by use of saturated aqueous ammonium chloride and ethyl acetate. The organic layer was dried over sodium sulfate anhydrate, followed by filtration. The solvent was removed under reduced pressure, and the residue was purified through silica gel column chromatography (hexane-ethyl acetate), to thereby give 1-(5-chloro-2-pyridyl)ethanone as a solid (3.26 g, 59%).

1. customThe reaction mixture was partitioned by use of saturated aqueous ammonium chloride and ethyl acetate
2. dry with materialThe organic layer was dried over sodium sulfate anhydrate
3. filtrationfollowed by filtration
4. customThe solvent was removed under reduced pressure
5. customthe residue was purified through silica gel column chromatography (hexane-ethyl acetate)