反应详情

温度

65 °C

A stirred mixture of 7-acetyl-5-chloroquinolin-8-yl trifluoromethanesulfonate (0.12 g, 0.34 mmol, from Example 47, Step 2), 3-methoxypiperidine (0.047 g, 0.41 mmol), palladium acetate (1.5 mg, 0.0068 mmol), (S)-(−)-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (6.3 mg, 0.010 mmol), and cesium carbonate (0.31 g, 0.95 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 MgSO4 and evaporated under reduced pressure. The residue was purified on silica gel (eluting with 0 to 10% methanol in dichloromethane) to give the desired product (37.3 mg, 34%). LCMS calculated for C17H20ClN2O2 (M+H)+: m/z=319.1; Found: 319.1.

1. temperatureThe mixture was cooled
2. filtrationfiltered
3. washThe filtrate was washed with brine
4. dry with materialdried over MgSO4
5. customevaporated under reduced pressure
6. customThe residue was purified on silica gel (eluting with 0 to 10% methanol in dichloromethane)