反应详情

2,4-Dibromo-5,7-difluoro-3-methylquinoline (2.00 g, 5.90 mmol), piperidin-2-one (590 mg, 5.90 mmol), copper (I) iodide (57.0 mg, 0.300 mmol), (1S,2S)—N1,N2-dimethylcyclohexane-1,2-diamine (0.094 mL, 0.59 mmol) and potassium phosphate tribasic (2.50 g, 11.9 mmol) were combined in 1,4-dioxane (10 mL) and stirred in a microwave reactor for 3.5 h. The reaction was diluted with water and extracted with EtOAc (2×100 mL). The combined organic layers were washed with brine and dried over MgSO4. The crude product was then purified by column chromatography (silica gel, 0 to 100% EtOAc:hexanes) to give 1-(4-bromo-5,7-difluoro-3-methylquinolin-2-yl)piperidin-2-one. Mass Spectrum (ESI) m/e=355.0 [(M+1) (79Br)] and 357.1 [(M+1) (81Br)].

1. extractionextracted with EtOAc (2×100 mL)
2. washThe combined organic layers were washed with brine
3. dry with materialdried over MgSO4
4. customThe crude product was then purified by column chromatography (silica gel, 0 to 100% EtOAc:hexanes)