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Amide bond formation is one of the most fundamental reactions in chemistry. Conventional amide synthesis faces challenges of poor atom economy and reliance on hazardous reagents. Herein, we present a tandem electro\u2010thermal catalytic pathway for the synthesis of acetamide from acetonitrile, leveraging electrochemically generated superoxide radicals to steer oxygen insertion under ambient conditions. The superoxide radicals were formed via controlled electroreduction of molecular oxygen. In 1\u00a0M K\n                    <jats:sub>2<\/jats:sub>\n                    CO\n                    <jats:sub>3<\/jats:sub>\n                    electrolyte containing methanol, we achieved over 94% selectivity toward acetamide at a total current density up to 104\u00a0mA cm\n                    <jats:sup>\u22122<\/jats:sup>\n                    , with a productivity of 878\u00a0\u00b5mol cm\n                    <jats:sup>\u22122<\/jats:sup>\n                    h\n                    <jats:sup>\u22121<\/jats:sup>\n                    . Mechanistic studies reveal that the superoxide radicals stabilized by a buffered alkaline environment facilitated the nucleophilic C\u2500O coupling at the nitrile group, while the presence of methanol quenched the hydroxyl radicals and effectively suppressed the over\u2010oxidation of acetamide to acetate. This coupled electro\u2010thermal catalysis enables the synthesis of a large variety of amides and may inspire more complex organic synthesis through active oxygen species\u2010mediated process.\n                  <\/jats:p>","DOI":"10.1002\/anie.202513359","type":"journal-article","created":{"date-parts":[[2025,9,11]],"date-time":"2025-09-11T12:11:38Z","timestamp":1757592698000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":15,"title":["Steering Amide Synthesis from Acetonitrile by Electrochemically Derived Active Superoxide"],"prefix":"10.1002","volume":"64","author":[{"given":"Ling\u2010Yu","family":"Dong","sequence":"first","affiliation":[{"name":"State Key Laboratory of Fine Chemicals Frontier Science Center for Smart Materials Liaoning Key Laboratory for Catalytic Conversion of Carbon Resources and School of Chemical Engineering Dalian University of Technology  Dalian 116024 P.R. 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China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5849-9965","authenticated-orcid":false,"given":"Guang\u2010Ping","family":"Hao","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Fine Chemicals Frontier Science Center for Smart Materials Liaoning Key Laboratory for Catalytic Conversion of Carbon Resources and School of Chemical Engineering Dalian University of Technology  Dalian 116024 P.R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"An\u2010Hui","family":"Lu","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Fine Chemicals Frontier Science Center for Smart Materials Liaoning Key Laboratory for Catalytic Conversion of Carbon Resources and School of Chemical Engineering Dalian University of Technology  Dalian 116024 P.R. 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