反应详情

1-(5'-(3"-t-butoxycarbonylaminopropyloxy)-2'-nitrophenyl)-2-propen-1-ol (9.66 g) is dissolved in chloroform (300 ml) and thereto is added activated manganese dioxide (7.2 g), and the mixture is heated with reflux. After completion of the reaction, inorganic materials are filtered off with celite, and the filtrate is concentrated, and thereto is added ethyl acetate. The organic layer is separated, washed with an aqueous saturated saline solution, dried over sodium sulfate. After distilling off the solvent, the residue is purified with a silica gel column chromatography to give 1-[5'-(3"-t-butoxycarbonylaminopropyloxy)-2'-nitrophenyl]-2-propen-1-one (6.01 g) as yellow color crystal.

1. temperaturethe mixture is heated
2. temperaturewith reflux
3. customAfter completion of the reaction, inorganic materials
4. filtrationare filtered off with celite
5. concentrationthe filtrate is concentrated
6. additionis added ethyl acetate
7. customThe organic layer is separated
8. washwashed with an aqueous saturated saline solution
9. dry with materialdried over sodium sulfate
10. distillationAfter distilling off the solvent
11. customthe residue is purified with a silica gel column chromatography