Electrocatalytic Defluorocarboxylation of Trifluoromethylbenzene With Carbon Dioxide

The study presents an electrocatalytic carboxylation strategy for synthesizing fluorinated organic compounds using CO 2 as a renewable C1 source. The process was optimized for maximum yield using trifluorotoluene as the model substrate. The experiments utilized a platinum cathode and magnesium anode in an N , N ‐dimethylformamide (DMF) solvent. Through response surface methodology, the influence of electrolyte types, electrode materials, and solvent systems was investigated. The highest yield of 90.0% was achieved under optimized conditions: using tetrabutylammonium bromide as the electrolyte, Mg–Pt electrodes, and DMF as solvent, with a reaction time of 5.8 h, a reaction current of 14.9 mA, and an electrolyte concentration of 0.08 mol/L. A plausible reaction mechanism was proposed on the basis of cyclic voltammetry (CV) measurements and radical trapping experiments, which involved the generation of fluorinated alkyl radical intermediates and their subsequent reaction with CO 2 . This green synthesis strategy provides an environmentally friendly and sustainable approach to producing high‐value fluorinated carboxylic acids, supporting global carbon neutrality goals.