反应详情

温度

80 °C

To a stirred solution of triphenylphosphine (126 mg, 0.48 mmol) in CCl4 (1 mL) at 0° C. was added triethylamine (67 μL, 0.48 mmol) and difluoroacetic acid (11 μL, 0.18 mmol). After 10 min, {1-[4-(7,8-diamino-4-oxo-2-phenyl-4H-chromen-3-yl)-phenyl]-cyclobutyl}-carbamic acid tert-butyl ester (80 mg, 0.16 mmol) in 1,2-dichloroethane (1 mL) was added, the temperature raised to 80° C. After 2.5 hours, the reaction mixture was allowed to cool to RT and the solution was directly subjected to flash chromatography (SiO2, 40% ethyl acetate in cyclohexane) to give the title compound as a pale yellow solid (64 mg, 72%). LCMS (Method G): RT=3.93 min, [M+H]+=558.

1. waitAfter 2.5 hours
2. temperatureto cool to RT