反应详情

To a solution of 2-chloro-6-(3-methoxyazetidin-1-yl)-4-(1-(oxetan-3-yl)piperidin-4-yl)pyridine (80 mg, 0.24 mmol), 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-3-(trifluoromethyl)pyridin-2-amine (140 mg, 0.48 mmol) and cesium carbonate (160 mg, 0.48 mmol) in dioxane/H2O (5:1, 4 mL) was added [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium (II) (18 mg, 0.024 mmol) under nitrogen. The mixture was irradiated by microwave at 110° C. for 30 min. The reaction mixture was filtered, the filtrate was concentrated and purified by Prep-HPLC to afford 6-(3-methoxyazetidin-1-yl)-4-(1-(oxetan-3-yl)piperidin-4-yl)-5′-(trifluoromethyl)-[2,3′-bipyridin]-6′-amine (68.3 mg 61.5%, yield). LCMS (ESI) [MH]+=464, 1HNMR (400 MHz, CDCl3), δ8.745(s,1H), δ8.363(s,1H), δ8.232(s,1H), δ8.832(s,1H), δ6.109(s,1H), δ5.642(s,2H), δ4.74- 4.67(m,4H), δ 4.39-4.22 (m, 3H), δ 3.94-3.90 (m, 2H), δ 3.63-3.56(m, 1H), δ 3.346(s, 3H), δ 2.980(d, J=10.8 Hz, 2H), δ 2.55-2.46 (m,1H), δ 2.06-1.99 (m, 1H), δ 1.93-1.87(m, 4H). LCMS:464.0(M+1).

1. customThe mixture was irradiated by microwave at 110° C. for 30 min
2. filtrationThe reaction mixture was filtered
3. concentrationthe filtrate was concentrated
4. custompurified by Prep-HPLC