反应详情

温度

100 °C

A vial was charged with 2-[(6-chloro-4-tetrahydropyran-4-yl-2-pyridyl)amino]pyridine-4-carbonitrile (51.1 mg, 0.162 mmol), [1,1-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (13.5 mg, 10 mol %), methylboronic acid (20.0 mg, 0.325 mmol), and potassium carbonate (68 mg, 0.49 mmol) and purged under nitrogen before the addition of degassed 1,4-dioxane (1.6 mL) and degassed water (0.5 mL). The mixture was stirred at 100° C. for 19 hr and then diluted with CH2Cl2, filtered through Celite and washed with brine. The organics were dried over MgSO4 and concentrated to dryness. The reaction residue thus obtained was purified by RPLC to afford 2-((6-methyl-4-(tetrahydro-2H-pyran-4-yl)pyridin-2-yl)amino)isonicotinonitrile as a white solid (4.1 mg, 9%); ESI-LRMS m/z [M+1]+=295.

1. custompurged under nitrogen before the addition of degassed 1,4-dioxane (1.6 mL)
2. customdegassed water (0.5 mL)
3. additiondiluted with CH2Cl2
4. filtrationfiltered through Celite
5. washwashed with brine
6. dry with materialThe organics were dried over MgSO4
7. concentrationconcentrated to dryness
8. customThe reaction residue thus obtained
9. customwas purified by RPLC