反应详情

HCl in dioxane (4M, 10 mL, 0.04 mol) was added to a solution of [(S)-1-(3-cyano-4-fluoro-2-phenylaminophenylcarbamoyl)propyl]carbamic acid tert-butyl ester (0.54 g, 1.32 mmol) in dioxane (5 mL) at 20° C., and the resultant mixture stirred at 80° C. for 17 h. After cooling, the reaction mixture was partitioned between saturated aqueous NaHCO3 (20 mL) and EtOAc (3×20 mL). The combined EtOAc extracts were dried (Na2SO4) and concentrated in vacuo. The resulting residue was purified by chromatography (SiO2 0-20% methanol in EtOAc) to give the title compound as an oil (0.27 g, 69%) LCMS (method H): RT 2.03 min, [M+H]+ 295.

1. temperatureAfter cooling
2. customthe reaction mixture was partitioned between saturated aqueous NaHCO3 (20 mL) and EtOAc (3×20 mL)
3. dry with materialThe combined EtOAc extracts were dried (Na2SO4)
4. concentrationconcentrated in vacuo
5. customThe resulting residue was purified by chromatography (SiO2 0-20% methanol in EtOAc)