The effectiveness of sulfated mesoporous niobium oxide (MNO-S) as a catalyst for the production of 5hydroxymethylfurfural (5-HMF) from sugar was studied and is reported herein. The structures of the synthesized MNO-S catalysts and commercial Nb 2 O 5 were characterized by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), Brunauer−Emmett−Teller (BET) analysis, and Fourier transform infrared (FTIR) spectroscopy. Compared with commercial Nb 2 O 5 , the MNO-S-based catalysts showed a much higher surface area and acidity. MNO-S calcined at 300 °C was found to be the most effective catalyst in fructose dehydration into 5-HMF in DMSO, with a yield as high as 88% and excellent recyclability. Furthermore, the Bronsted acid sites on the surface of the catalyst enable hydrolysis and dehydration reactions to occur in a one-pot manner. As such, MNO-S effectively transforms a wide range of sugar substrates, such as sucrose, cellobiose, and even the polysaccharide inulin, into 5-HMF with reasonable yields.