反应详情

Lithium hydride (52 mg, 6.5 mmol) was added to a solution of 6,7-difluoroquinoxalin-2(1H)one (1 g, 5.4 mmol) in N,N-dimethylformamide (10 ml) under cooling on ice and the reaction mixture was stirred at room temperature for 30 minutes. The mixture was cooled on ice again, a solution of 2-(2-bromoethyl)-1,3-dioxolane (0.8 ml, 6.5 mmol) in N,N-dimethylformamide (2 ml) was gradually added thereto and the obtained mixture was stirred for 4 hours. Water was gradually added to the reaction solution and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and the solvent was removed under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to yield 0.6 g (39%) of the title compound.

1. temperatureunder cooling on ice
2. temperatureThe mixture was cooled on ice again
3. stirringthe obtained mixture was stirred for 4 hours
4. extractionthe mixture was extracted with ethyl acetate
5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
6. customthe solvent was removed under reduced pressure
7. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate)