反应详情

To a solution of 4-(4-bromo-2,3-difluorophenyl)-N,2-dimethylnicotinamide (600 mg, 1.76 mmol) in tetrahydrofuran (20 mL) at 0° C. was added NaH (176 mg, 4.40 mmol) and the reaction mixture was brought to room temperature gradually. The reaction mixture was stirred at room temperature for 15 h. The reaction mixture was diluted with water (50 mL) and extracted with ethyl acetate (100 mL). The organic layer was separated, dried over Na2SO4 and concentrated under reduced pressure to afford 8-bromo-7-fluoro-4,6-dimethylbenzo[c][2,7]naphthyridin-5(6H)-one (400 mg, 1.24 mmol, 71% yield) as yellow solid. LC/MS (ESI) m/e 322.8 [(M+2H)+, calcd for C14H12BrFN2O 322.9]; LC/MS retention time (method G): tR=2.21 min.

1. customwas brought to room temperature
2. extractionextracted with ethyl acetate (100 mL)
3. customThe organic layer was separated
4. dry with materialdried over Na2SO4
5. concentrationconcentrated under reduced pressure