反应详情

温度

65 °C

A stirred mixture of 7-acetyl-5-chloroquinolin-8-yl trifluoromethanesulfonate (0.106 g, 0.301 mmol), 4,4-difluoropiperidine hydrochloride (0.0570 g, 0.362 mmol), palladium acetate (1 mg, 0.006 mmol), (S)-(−)-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (6 mg, 0.009 mmol), and cesium carbonate (0.274 g, 0.843 mmol) in tetrahydrofuran (3 mL) was heated at 65° C. overnight. The mixture was cooled, diluted with dichloromethane and filtered. The filtrate was washed with brine, dried over sodium sulfate and evaporated to dryness. The resulting residue was purified on silica gel, eluting with 0 to 50% ethyl acetate in hexane, to give the desired product. LCMS calculated for C16H16ClF2N2O (M+H)+: m/z=325.1; Found: 325.0.

1. temperatureThe mixture was cooled
2. filtrationfiltered
3. washThe filtrate was washed with brine
4. dry with materialdried over sodium sulfate
5. customevaporated to dryness
6. customThe resulting residue was purified on silica gel
7. washeluting with 0 to 50% ethyl acetate in hexane