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Herein, we propose a catalyst cascade Scheme in which CO<jats:sub>2<\/jats:sub> is used as a CO surrogate in the carbonylation of benzyl chlorides. Our approach is based on the cooperation between two coexisting catalytic cycles: the CO<jats:sub>2<\/jats:sub>\u2010to\u2010CO electroreduction cycle promoted by [Fe(TPP)Cl] (TPP=meso\u2010tetraphenylporphyrin) and an electrochemical carbonylation cycle catalyzed by [Ni(bpy)Br<jats:sub>2<\/jats:sub>] (2,2\u2032\u2010bipyridine). As a proof of concept, this protocol allows for the synthesis of symmetric ketones from good to excellent yields in an undivided cell with non\u2010sacrificial electrodes. The reaction can be directly scaled up to gram\u2010scale and operates effectively at a CO<jats:sub>2<\/jats:sub> concentration of 10\u2009%, demonstrating its robustness. Our mechanistic studies based on cyclic voltammetry, IR spectroelectrochemistry and Density Functional Theory calculations suggest a synergistic effect between the two catalysts. The CO produced from CO<jats:sub>2<\/jats:sub> reduction is key in the formation of the [Ni(bpy)(CO)<jats:sub>2<\/jats:sub>], which is proposed as the catalytic intermediate responsible for the C\u2212C bond formation in the carbonylation steps.<\/jats:p>","DOI":"10.1002\/anie.202403674","type":"journal-article","created":{"date-parts":[[2024,4,22]],"date-time":"2024-04-22T13:09:13Z","timestamp":1713791353000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":25,"title":["An Electrocatalytic Cascade Reaction for the Synthesis of Ketones Using CO<sub>2<\/sub> as a CO Surrogate"],"prefix":"10.1002","volume":"63","author":[{"given":"Ahmed M.","family":"Sheta","sequence":"first","affiliation":[{"name":"Institute of Chemical Research of Catalonia (ICIQ) Barcelona Institute of Science and Technology  Avda. Pa\u00efsos Catalans, 16 43007 Tarragona Spain"},{"name":"Departament de Qu\u00edmica Org\u00e0nica i Anal\u00edtica Universitat Rovira i Virgili  Carrer Marcel\u2009\u22c5\u2009l\u00ed Domingo s\/n 43007 Tarragona Spain"},{"name":"Department of Chemistry Damietta University  Damietta El-Gadeeda City, Kafr Saad, Damietta Governorate 34511 Egypt"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Sergio","family":"Fern\u00e1ndez","sequence":"additional","affiliation":[{"name":"Institute of Chemical Research of Catalonia (ICIQ) Barcelona Institute of Science and Technology  Avda. Pa\u00efsos Catalans, 16 43007 Tarragona Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Changwei","family":"Liu","sequence":"additional","affiliation":[{"name":"Institute of Chemical Research of Catalonia (ICIQ) Barcelona Institute of Science and Technology  Avda. 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