反应详情

温度

100 °C

To a nitrogen purged vessel was added Pd2 dba3 (0.0386 g, 0.0422 mmol), NaOtBu (0.169 g, 1.76 mmol), 2,8,9-triisobutyl-2,5,8,9-tetraaza-1-phosphabicyclo[3.3.3]undecane (0.0600 mL, 0.169 mmol), 2-chloro-5-ethylpyridine (0.100 g, 0.703 mmol) and (S)-3-(2-fluoro-4-(methylsulfonyl)phenylamino)-1-(piperidin-4-yl)pyrrolidin-2-one (Preparation E; 0.300 g, 0.844 mmol). Toluene (4 mL, purged with nitrogen) was added and the reaction was heated at 100° C. overnight. The mixture was cooled to ambient temperature, diluted with EtOAc, and washed with water. The organics were dried over Na2SO4, concentrated and purified on silica eluting with 100% EtOAc to give 1-(1-(5-ethylpyridin-2-yl)piperidin-4-yl)-3-(2-fluoro-4-(methylsulfonyl)phenylamino)pyrrolidin-2-one (0.177 g, 54% yield) as white solids. Mass spectrum (apci) m/z=461.3 (M+H).

1. temperatureThe mixture was cooled to ambient temperature
2. washwashed with water
3. dry with materialThe organics were dried over Na2SO4
4. concentrationconcentrated
5. custompurified on silica eluting with 100% EtOAc