反应详情

To a solution of tert-butyl 3,6-dihydropyridine-1(2H)-carboxylate (617 g, 3.37 mol) in anhydrous DCM (10 L) was added m-CPBA (989 g, 5.73 mol) in portions at 0° C. The mixture was stirred at room temperature for 1 hour. Saturated Na2S2O3 (1 L) was added and the organic layer was separated. The organic layer was washed with 5% aqueous K2CO3 (5 L×2), brine (4 L), dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by column chromatography (petroleum ether:ethyl acetate=100:1-20:1) to obtain pure tert-butyl 7-oxa-3-azabicyclo[4.1.0]heptane-3-carboxylate.

1. customthe organic layer was separated
2. washThe organic layer was washed with 5% aqueous K2CO3 (5 L×2), brine (4 L)
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by column chromatography (petroleum ether:ethyl acetate=100:1-20:1)