反应详情

To a solution of (3R,4R)-tert-butyl 3-azido-4-hydroxypyrrolidine-1-carboxylate (2.00 g, 8.76 mmol) and MeI (1.64 mL, 26.3 mmol) in DMF (20 mL) was added 60% NaH (0.701 g, 17.5 mmol) at 0° C. The mixture was warmed to ambient temperature and stirred at ambient temperature for 1 hour. Water (20 mL) and ether (40 mL) were added. The organic layer was separated, washed with brine, dried (sodium sulfate), filtered and concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel (3:1 hexane/ethyl acetate) to give (3R,4R)-tert-butyl 3-azido-4-methoxypyrrolidine-1-carboxylate (2.04 g, 96.1%) as thick oil.

1. customThe organic layer was separated
2. washwashed with brine
3. dry with materialdried (sodium sulfate)
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by flash chromatography on silica gel (3:1 hexane/ethyl acetate)