The condensation of 4-demethoxy-doxorubicinone acetate (I) with the protected disaccharide p-nitrobenzoate (II) in the presence of trimethylsilyl triflate afforded adduct (III). The acetate ester of (III) was then hydrolyzed by treatment with K2CO3 in methanol/dichloromethane affording alcohol (IV). Finally, deprotection of the allyloxycarbonyl groups of (IV) employing palladium tetrakis(triphenylphosphine) gave rise to the title compound.