A surface modification approach has prepared a nanostructured organic framework connecting two metal oxide NPs. The surface modifier attached two metal oxide NPs <em>via</em> molecular interaction to generate modular structures of fiber, rod, or sponge materials. Thus, obtained hybrid systems have been confirmed through FT-IR, TGA, PXRD, and SEM. Metal oxides such as Fe<sub>3</sub>O<sub>4</sub> and MgO generated mixed materials via the surface modification approach. Thus, obtained materials have been successfully used to dehydrate biomass-derived glucose. The products HMF and subsequently partially oxidized product DFF are considered to be valuable compounds not only in fuel technology but also in the pharmaceutical industry.