反应详情

To a stirred solution at 0° C. of N--t-Butoxycarbonyl-O-benzylhydroxylamine, prepared as in Example 1175A, in anhydrous THF was added portionwise a 60% dispersion of sodium hydride (1.2 equiv.) in mineral oil. Mixture stirred 30 minutes ar 0° C., and then, 1-iodobutane (1.2 equiv.) was added dropwise. Reaction stirred one hour at 0° C., and than, overnight at room temperature. Reaction concentrated in vacuo. Residue taken up in EtOAc and washed with water, 1.0M NaHCO3, 1N H3PO4, and brine. Organic layer dried with Na2SO4, filtered, and evaporated.

1. customar 0° C.
2. customReaction
3. stirringstirred one hour at 0° C.
4. customovernight
5. customat room temperature
6. customReaction
7. concentrationconcentrated in vacuo
8. washwashed with water, 1.0M NaHCO3, 1N H3PO4, and brine
9. dry with materialOrganic layer dried with Na2SO4
10. filtrationfiltered
11. customevaporated