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The aqueous room temperature mono-dehydration of sugar alcohols (D-sorbitol and D-mannitol) was conducted using functionalized yttrium oxide nanocatalysts prepared via sol-gel methods. Materials exhibited high selectivity to mono-dehydration products. Solvent and catalyst effects were also investigated and discussed. The introduction of titanium into the yttrium oxide framework would decrease both substrate conversion and mono-dehydration efficiency. In addition, studies of the catalytic mechanism indicate high mono-dehydration efficiency may come from the stability of the formed intermediate during catalysis. This work provides a highly efficient and benign system for catalytic mono-dehydration of sugar alcohols.