反应详情

1.02 g (2.92 mmol) of Compound 27 obtained in Example 27 was dissolved in 25 ml of dimethylformamide under argon atmosphere, 129 mg of sodium hydride (60% oil dispersion) and 2.9 ml of 1-bromo-3-chloropropane were added under ice-cooling and the mixture was stirred at room temperature for 1 hour. Water was added to the reaction solution and the mixture was extracted twice with ethyl acetate. The organic layer was washed once with water and once with an aqueous saturated solution of sodium chloride and dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. Recrystallization from ethyl acetate/acetonitrile afforded 434 mg (35%) of 2-[4-[N-acetyl-N-(3-chloropropyl)amino]-3-fluorophenyl]-5-amino-6,8-difluoro-4H-1-benzopyran-4-one.

1. temperaturecooling
2. extractionthe mixture was extracted twice with ethyl acetate
3. washThe organic layer was washed once with water and once with an aqueous saturated solution of sodium chloride
4. dry with materialdried over anhydrous sodium sulfate
5. distillationthe solvent was distilled off under reduced pressure
6. customRecrystallization from ethyl acetate/acetonitrile