反应详情

温度

60 °C

(S)-1-(1-(5-Chloropyrazin-2-yl)piperidin-4-yl)-3-(2-fluoro-5-methyl-4-(methylsulfonyl)phenylamino)pyrrolidin-2-one (Example 1; 320 mg, 0.664 mmol) was dissolved in THF (6 mL) and K2CO3 (275 mg, 1.99 mmol) and PdCl2(dppf)*CH2Cl2 (54.2 mg, 0.0664 mmol) were added and purged with nitrogen. Diethylzinc (1 M in THF; 797 μL, 0.797 mmol) was added and the reaction heated to 60° C. for 1 hour. The reaction was cooled to ambient temperature, partitioned between water and EtOAc, dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified over silica gel (100% EtOAc) to afford (S)-1-(1-(5-ethylpyrazin-2-yl)piperidin-4-yl)-3-(2-fluoro-5-methyl-4-(methylsulfonyl)phenylamino)pyrrolidin-2-one (175 mg, 0.368 mmol, 55.4% yield) as a tan solid. Mass spectrum (apci) m/z=476.3 (M+H).

1. custompurged with nitrogen
2. temperatureThe reaction was cooled to ambient temperature
3. custompartitioned between water and EtOAc
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe residue was purified over silica gel (100% EtOAc)