反应详情

温度

60 °C

To a solution of methyl 2-(2-(2-chloro-5-((2S,3S,4R,5R,6R)-3,4,5-tris(benzyloxy)-6-(benzyloxymethyl)tetrahydro-2H-pyran-2-yl)phenyl)acetamido)acetate (compound 54, 1.1 g, 1.44 mmol) in MeOH (20 ml) was added hydrazine anhydrous (2 ml) at room temperature. Then, the reaction temperature was raised to 60° C., and maintained for overnight. After reaction complete, the solution was evaporated in vacuo, and the residue was dissolved in acetic acid (10 ml) with ammonium acetate (1 g). The reaction solution was refluxed for 1 day. The resulting solution was cooled to room temperature, and then evaporated under reduced pressure. The residue was purified with column chromatography (Hx/EtOAc=1/1) to afford to title compound (826 mg, 77% overall yield) as white solid.

1. temperaturemaintained for overnight
2. customAfter reaction complete
3. customthe solution was evaporated in vacuo
4. dissolutionthe residue was dissolved in acetic acid (10 ml) with ammonium acetate (1 g)
5. temperatureThe reaction solution was refluxed for 1 day
6. temperatureThe resulting solution was cooled to room temperature
7. customevaporated under reduced pressure
8. customThe residue was purified with column chromatography (Hx/EtOAc=1/1)