反应详情

温度

0 °C

To a solution of 4-(2-fluoropyridin-3-yl)pyrrolidin-2-one (0.254 g, 1.41 mmol) in DMF (5 mL) at 0° C. was added iodomethane (0.090 mL, 1.4 mmol) and sodium hydride (60% weight dispersion in mineral oil, 0.056 g, 1.4 mmol). The reaction mixture was stirred at 0° C. for 30 min, warmed to room temperature, and stirred for 30 min. The reaction mixture was diluted with EtOAc, quenched with water, and diluted with brine and water. The aqueous phase was extracted with EtOAc (6×) and the combined organic extracts were washed with brine (1×), dried over MgSO4, filtered, and concentrated. Purification by flash column chromatography on silica gel (50% to 100% EtOAc (10% MeOH) in hexanes) gave 4-(2-fluoropyridin-3-yl)-1-methylpyrrolidin-2-one as a pale yellow oil. MS (ESI, pos. ion) m/z: 195.1 (M+1).

1. temperaturewarmed to room temperature
2. stirringstirred for 30 min
3. customquenched with water
4. additiondiluted with brine and water
5. extractionThe aqueous phase was extracted with EtOAc (6×)
6. washthe combined organic extracts were washed with brine (1×)
7. dry with materialdried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated
10. customPurification by flash column chromatography on silica gel (50% to 100% EtOAc (10% MeOH) in hexanes)