反应详情

To a methanol (2.6 mL)-ethyl acetate (1.3 mL) mixture solution of (1S)-1-[5-[4-[(1E)-3-[[benzyloxy carbonyl amino(benzyloxycarbonylimino)methyl]amino]prop-1-en-1-yl]benzyl]-2-(benzyloxy)-4-methylphenyl]-1,5-anhydro-2,3,4,6-tetra-O-benzyl-D-glucitol (154 mg, 0.131 mmol) was added 20% palladium hydroxide (160 mg), and the mixture was stirred under a hydrogen atmosphere at room temperature overnight. The reaction solution was filtered through celite, and evaporated under reduced pressure to obtain a residue. Thus obtained residue was dissolved in methanol (1.5 mL). And 20% palladium hydroxide (63 mg) was added thereto, and the mixture was stirred under a hydrogen atmosphere at room temperature for 2 days. The reaction solution was filtered through celite, and evaporated under reduced pressure to obtain a residue. Thus obtained residue was purified with silica gel column chromatography (ethyl acetate:ethanol:water=10:2:1 then 5:2:1, and then ethanol:water=10:1) to obtain the title compound (38 mg, 63%) as a colorless powder. NMR data and MS data of the compound are shown in Table 1.

1. filtrationThe reaction solution was filtered through celite
2. customevaporated under reduced pressure
3. customto obtain a residue
4. stirringthe mixture was stirred under a hydrogen atmosphere at room temperature for 2 days
5. filtrationThe reaction solution was filtered through celite
6. customevaporated under reduced pressure
7. customto obtain a residue
8. customThus obtained residue was purified with silica gel column chromatography (ethyl acetate