反应详情

To a solution of 1-bromo-3,5-difluorobenzene (3.13 g, 16.2 mmol) in dry tetrahydro-furan (40 mL), under nitrogen, was added magnesium turnings (0.39 g, 16.2 mmol). The mixture was refluxed for 1 h, cooled to ambient temperature and a solution of 1-N-boc-3-pyrrolidinone (2.0 g, 10.8 mmol) in dry tetrahydrofuran (10 mL) was added drop wise. The resulting mixture was refluxed 1 h, cooled to ambient temperature, aqueous saturated ammonium chloride solution (40 mL) was added and the mixture was extracted with ethyl acetate (3×50 mL). The combined organic phase was dried (MgSO4), filtered and evaporated to give the title compound (3.38 g). MS m/z (rel. intensity, 70 eV) 299 (M+, 1), 243 (42), 198 (49), 168 (31), 127 (28), 57 (bp).

1. temperatureThe mixture was refluxed for 1 h
2. temperatureThe resulting mixture was refluxed 1 h
3. temperaturecooled to ambient temperature
4. extractionthe mixture was extracted with ethyl acetate (3×50 mL)
5. dry with materialThe combined organic phase was dried (MgSO4)
6. filtrationfiltered
7. customevaporated