反应详情

A DCM (12 mL) solution of TFA (11.3 mL, 146 mmol) was added to (R)-tert-butyl 2-(5-fluoro-2-methoxypyridin-3-yl)pyrrolidine-1-carboxylate (4.33 g, 14.6 mmol) and stirred at ambient temperature for 1 hour. The reaction was then concentrated, taken up in EtOAc, then washed with NaHCO3 and brine. The organic phase was dried (MgSO4), filtered, and concentrated, and the crude material was purified by silica column chromatography eluting with a 1-2% 7 N NH3-MeOH/DCM to afford (R)-5-fluoro-2-methoxy-3-(pyrrolidin-2-yl)pyridine as a liquid (1.40 g, 49% yield).

1. concentrationThe reaction was then concentrated
2. washwashed with NaHCO3 and brine
3. dry with materialThe organic phase was dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated
6. customthe crude material was purified by silica column chromatography
7. washeluting with a 1-2% 7 N NH3-MeOH/DCM