反应详情

温度

83 °C

To a stirred solution of N2′-(trans-4-aminocyclohexyl)-5′-chloro-5-fluoro-N6-((tetrahydro-2H-pyran-4-yl)methyl)-2,4′-bipyridine-2′,6-diamine (90 mg, 0.207 mmol)) in DMSO (1.0 ml) was add potassium carbonate (71.7 mg, 0.518 mmol), followed by follow oxetan-2-yl-methyl 4-methylbenzenesulfonate (151 mg, 0.622 mmol). The mixture was heated at 83° C. for 2 h. The mixture was allowed to cool to ambient temperature, then diluted with water and then extracted with EtOAc (×3). The organics were combined then washed with water (×2), saturated brine (×2), then dried (Na2SO4), filtered and evaporated under reduced pressure. The resulting residue was purified by reverse phase prep HPLC and lyophilized to yield titled compound. LCMS (m/z): 504.4/506.5 (MH+) retention time=0.60 min as a TFA salt.

1. temperatureto cool to ambient temperature
2. extractionextracted with EtOAc (×3)
3. washThe organics were combined then washed with water (×2), saturated brine (×2)
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. customevaporated under reduced pressure
7. customThe resulting residue was purified by reverse phase prep HPLC