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Herein, we present an integrated upper division chemistry laboratory experiment involving the synthesis, characterization, and evaluation of catalytic metal–organic frameworks (MOFs). Experiments are designed to facilitate the solvothermal synthesis and characterize MOFs, including UiO-66, UiO-66-NH2, and UiO-66-NO2. The MOFs are employed as catalysts in oxidative desulfurization (ODS) of an organic sulfur-containing compound, dibenzothiophene (DBT), in a laboratory experiment. To investigate the composition and structure of the MOFs, powder X-ray diffraction (PXRD) and elemental analysis (EA), respectively, are employed. Using Fourier transform infrared (FT-IR) spectroscopy, students evaluate the different organic linkers found in the MOFs. Students then investigate the effects of the electronic environment of the organic linker of the MOFs on the ODS of DBT. Students find that all three porous and crystalline MOFs oxidize DBT, but UiO-66-NO2 exhibits the most efficient catalytic conversion.