反应详情

温度

110 °C

To a scintillation vial was added 3,5′-dichloro-2′-fluoro-N-((tetrahydro-2H-pyran-4-yl)methyl)-2,4′-bipyridin-6-amine (25 mg, 0.070 mmol), racemic tert-butyl trans-4-aminocyclohexyl(tetrahydrofuran-3-yl)carbamate (21.95 mg, 0.077 mmol), DIPEA (24.51 μl, 0.140 mmol) and NMP (0.2 ml). This was heated at 110° C. for 48 h. The mixture was diluted with EtOAc and washed with water (×2), saturated brine (×2), then dried (Na2SO4), filtered and evaporated under reduced pressure. The resulting residue was dissolved in CH2Cl2 (0.4 mL) and treated with TFA (100 μl, 1.298 mmol). After 30 minutes, the mixture was concentrated in vacuo and the resulting residue was purified by reverse phase preparative HPLC and then lyophilized to yield racemic 3,5′-dichloro-N6-((tetrahydro-2H-pyran-4-yl)methyl)-N2′-(trans-4-(tetrahydrofuran-3-yl-amino)cyclohexyl)-2,4′-bipyridine-2′,6-diamine (10.8 mg), LCMS (m/z): 520.1/522.0 (bis-chloro isotopic signature for MH+), retention time=0.59 min as a TFA salt.

1. washwashed with water (×2), saturated brine (×2)
2. dry with materialdried (Na2SO4)
3. filtrationfiltered
4. customevaporated under reduced pressure
5. dissolutionThe resulting residue was dissolved in CH2Cl2 (0.4 mL)
6. concentrationthe mixture was concentrated in vacuo
7. customthe resulting residue was purified by reverse phase preparative HPLC