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A novel porous metal–organic framework Co(btc)(bpy) (Co-MOF-3a) was synthesized by employing a bipyridyl ligand, benzene tricarboxylic acid, and Co(NO3)2·6H2O and was completely characterized. The mesoporous nature of the MOF catalyst was confirmed using BET measurements. The confirmation of the proposed structure of Co-MOF-3a was also supported through a computational study. This MOF could serve as a highly efficient heterogeneous catalyst for the oxidation of a variety of alcohols with tert-butyl hydroperoxide (t-BuOOH) as an oxidant. Furthermore, the current catalytic approach facilitated the oxidative coupling reaction in one pot to obtain a wide range of biologically important molecules, such as benzimidazole, benzothiazole, quinozolones, and arylidene malononitrile. The high performance of the MOF could be due to the presence of both the metal and carboxylate group of the ligand. The recyclability and scalability of the catalyst was found to be efficient and suitable for commercial applications. [ABSTRACT FROM AUTHOR]