反应详情

To a solution of (±)-1,1-dimethylethyl cis-3-fluoro-4-[({[(phenylmethyl)oxy]carbonyl}amino)methyl]-1-pyrrolidinecarboxylate (0.45 g, 1.28 mmole) in DCM (50 mL) at RT was added TFA (25 mL). After 2 h, the reaction solution was concentrated under vacuum and the residue placed under high vacuum for 3 hr. The residue was dissolved in DCM (200 mL) and MP-carbonate resin (5.12 mmole, 1.9 g) was added with vigorous stirring at RT. After 4 h, the reaction contents were filtered through a scintered-glass funnel washing with MeOH (100 mL). The filtrate was concentrated under vacuum to give the title compound (0.32 g, 99%) as a light orange oil: LC-MS (ES) m/e 253 (M+H)+.

1. concentrationthe reaction solution was concentrated under vacuum
2. waitthe residue placed under high vacuum for 3 hr
3. dissolutionThe residue was dissolved in DCM (200 mL)
4. waitAfter 4 h
5. customthe reaction contents
6. filtrationwere filtered through a scintered-glass funnel
7. washwashing with MeOH (100 mL)
8. concentrationThe filtrate was concentrated under vacuum