反应详情

温度

80 °C

To a stirred solution of triphenylphosphine (126 mg, 0.48 mmol) in CCl4 (2 mL) at 0° C. was added triethylamine (67 μL, 0.48 mmol) and TFA (13 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) was added and the temperature raised to 80° C. After 2 hours, 1,2-dichloroethane (1 mL) was added to aid solubility. The reaction mixture was stirred for a further 1 hour before cooling to RT. The solution was directly subjected to flash chromatography (SiO2, 40% ethyl acetate in cyclohexane) to give the title compound as an off-white solid (38 mg, 41%). LCMS (Method H): RT=4.20 min, [M+H]+=576.

1. waitAfter 2 hours
2. temperaturebefore cooling to RT