Electrode Development for Electro‐Organic Kolbe–Schmitt C–H Carboxylation of Benzene Using Cu Nanoparticles on Graphene Oxide Modified With MIL‐101 MOF for CO₂ Capture in a DES Electrolyte System

ABSTRACT This study focuses on developing an advanced electrode for the electro‐organic Kolbe–Schmitt C–H carboxylation of benzene. The electrode uses copper (Cu) nanoparticles supported on graphene oxide modified with MIL‐101 metal–organic framework (MOF). The MIL‐101 MOF enhances CO 2 capture, improving the electrode's efficiency in a deep eutectic solvent (DES) system. The study reports high yields (89%–97%) of synthesized benzoic acids 4(a–l) , facilitated by urea/ChCl as a cost‐effective electrolyte, by applying an electric current of 20 mA, in 2 h and at ambient temperature. The innovative electrode design facilitates efficient benzoic acid synthesis, while the use of urea/ChCl as an accessible and cost‐effective electrolyte and solvent enhances the electro‐organic reaction rate. The synthesized benzoic acids were characterized through melting point analysis, 1 HNMR spectroscopy, and CHN elemental composition. To assess the electrode's properties, extensive characterization techniques such as XPS, TGA, SEM, EDS, FT‐IR, BET surface area analysis, CV, and FT‐IR were used.