反应详情

温度

95 °C

Treat a N2 degassed mixture of (S)-tert-butyl 4-(6-chloro-4,5-dimethylpyridazin-3-yl)-2-methylpiperazine-1-carboxylate (3.03 g, 8.87 mmol), phenylboronic acid (1.62 g, 13.3 mmol), and CsF (4.09 g, 26.9 mmol) in 1,4-dioxane (120 mL) with (1,1′-bis(diphenylphosphino)ferrocene)palladium(II) chloride (1.08 g, 1.32 mmol). Heat the reaction mixture at 95° C. overnight. Cool the reaction, and partition between EtOAc and H2O. Wash the organic layer with brine, dry over Na2SO4, filter, and concentrate under reduced pressure. Purify the residue by flash silica gel chromatography (gradient of 15 to 85% EtOAc in hexanes) to afford the title compound as a white solid (2.93 g, 86%). ES/MS m/z 383.0 (M+1).

1. customdegassed
2. temperatureCool
3. customthe reaction
4. custompartition between EtOAc and H2O
5. washWash the organic layer with brine
6. dry with materialdry over Na2SO4
7. filtrationfilter
8. concentrationconcentrate under reduced pressure
9. customPurify the residue by flash silica gel chromatography (gradient of 15 to 85% EtOAc in hexanes)