反应详情

温度

100 °C

6-Acetyl-3-chloro-pyridine-2-carbonitrile (64) (1.80 g, 9.97 mmol) was dissolved in MeCN (19 mL). (S)-3-Pyrrolidinol (884 μL, 10.9 mmol) and TEA (4.16 mL, 29.8 mmol) were added and the mixture stirred at 100° C. in the microwave for 20 minutes. The solvent was evaporated in vacuo and the crude material dissolved in EtOAc (100 mL). The solution was washed with 1:1 saturated brine solution-H2O (100 mL), saturated brine solution (100 mL), then dried (MgSO4), filtered and the solvent evaporated in vacuo. The crude product was purified by flash chromatography (Biotage SP1, 50 g SNAP cartridge) eluting with 6:4 isohexane-EtOAc→8:2 EtOAc-isohexane to yield the title compound as a yellow solid (1.32 g, 64%); LCMS, Rt=2.04 min (MeOH-FA method), m/z 232 (MH+).

1. customThe solvent was evaporated in vacuo
2. dissolutionthe crude material dissolved in EtOAc (100 mL)
3. washThe solution was washed with 1:1 saturated brine solution-H2O (100 mL), saturated brine solution (100 mL)
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customthe solvent evaporated in vacuo
7. customThe crude product was purified by flash chromatography (Biotage SP1, 50 g SNAP cartridge)
8. washeluting with 6:4 isohexane-EtOAc→8:2 EtOAc-isohexane