Ametal-organic framework (MOF)-based catalyst, chromium hydroxide/MIL-101(Cr), was prepared by aone-pot synthesis method. The combination of chromium hydroxide particles on and within Lewis acidic MIL-101 accomplishes highly selective conversion of glucose to fructose in the presence of ethanol, matching the performance of optimized Sn-containing Lewis acidic zeolites.D ifferently from zeolites, NMR spectroscopystudies with isotopically labeled molecules demonstrate that isomerization of glucose to fructose on this catalyst, proceeds predominantly via ap roton transfer mechanism.