反应详情

温度

65 °C

A stirred mixture of 5-chloro-7-{[methoxy(methyl)amino]carbonyl}quinolin-8-yl trifluoromethanesulfonate (0.150 g, 0.376 mmol), (3R)-pyrrolidin-3-ol (0.0394 g, 0.452 mmol, Aldrich), palladium acetate (2 mg, 0.008 mmol), 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (7 mg, 0.01 mmol), and cesium carbonate (0.343 g, 1.05 mmol) in tetrahydrofuran (4 mL) was heated at 65° C. overnight. The mixture was cooled, diluted with dichloromethane, washed with brine, dried over sodium sulfate, and evaporated to dryness. The resultant residue was purified on silica gel, eluting with 0 to 10% MeOH in dichloromethane, to give the desired product (115 mg, 91%). LCMS calculated for C16H19ClN3O3(M+H)+: m/z=336.1; found: 336.1.

1. temperatureThe mixture was cooled
2. washwashed with brine
3. dry with materialdried over sodium sulfate
4. customevaporated to dryness
5. customThe resultant residue was purified on silica gel
6. washeluting with 0 to 10% MeOH in dichloromethane