反应详情

5-Bromo-2-chloro-nicotinonitrile (6) (5.0 g, 23.0 mmol) was dissolved in MeCN (100 mL). (S)-3-Fluoropyrrolidine hydrochloride (5.7 g, 53.0 mmol) and DIPEA (12.0 mL, 68.9 mmol) were added and the mixture was stirred at reflux for 1 hour. The solvent was evaporated in vacuo and the residue partitioned between EtOAc (100 mL) and H2O (50 mL). The layers were separated and the organic phase washed with saturated brine solution (50 mL), then dried (MgSO4), filtered and the solvent evaporated in vacuo. The title compound was obtained as an off-white solid (6.2 g, 100%); LCMS, Rt=2.91 min (MeOH-FA method), m/z 270, 272 (MH+).

1. temperatureat reflux for 1 hour
2. customThe solvent was evaporated in vacuo
3. customthe residue partitioned between EtOAc (100 mL) and H2O (50 mL)
4. customThe layers were separated
5. washthe organic phase washed with saturated brine solution (50 mL)
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. customthe solvent evaporated in vacuo