反应详情

To a solution of (3R,4R)-tert-butyl 3-(benzyloxycarbonylamino)-4-hydroxypyrrolidine-1-carboxylate (4.91 g, 14.60 mmol) in DCM (20 mL) was added TFA (11.25 mL, 146.0 mmol) and the mixture was stirred at ambient temperature for 1 hour. The solvent was removed under reduced pressure. 6 N HCl in water (10 mL) was added. The mixture was stirred at ambient temperature for 30 minutes and neutralized with saturated sodium bicarbonate to about pH 8. It was extracted with DCM:IPA=4:1 (50 mL). The organic layer was separated, dried (sodium sulfate), filtered and concentrated under reduced pressure to give benzyl (3R,4R)-4-hydroxypyrrolidin-3-ylcarbamate (2.45 g, 71.0%) as a solid.

1. customThe solvent was removed under reduced pressure
2. addition6 N HCl in water (10 mL) was added
3. stirringThe mixture was stirred at ambient temperature for 30 minutes
4. extractionIt was extracted with DCM
5. customThe organic layer was separated
6. dry with materialdried (sodium sulfate)
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure