反应详情

To a solution of 3-(2-fluoropyridin-3-yl)cyclopent-2-enone (1 g, 5.64 mmol) in THF (28.2 mL) was added methylmagnesium bromide (4.70 mL, 14.11 mmol) dropwise over 5 minutes. The dark brown solution was stirred for 3 h at room temperature before. slowly quenching with aqueous ammonium chloride. The crude reaction was diluted with water and extracted with ethyl acetate, drying over magnesium sulfate, filtering, and concentrating to a dark brown oil under reduced pressure. The crude compound was purified by column chromatography (ethyl acetate/dichloromethane) to afford 3-(2-fluoropyridin-3-yl)-1-methylcyclopent-2-enol as a clear oil. MS (ESI, pos. ion) m/z: 194.1 (M+1).

1. customslowly quenching with aqueous ammonium chloride
2. customThe crude reaction
3. extractionextracted with ethyl acetate
4. dry with materialdrying over magnesium sulfate
5. filtrationfiltering
6. concentrationconcentrating to a dark brown oil under reduced pressure
7. customThe crude compound was purified by column chromatography (ethyl acetate/dichloromethane)