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Catalyst design strategies that spatially arrange discrete active sites, analogous to relay runners, facilitate the sequential activation of reaction steps, thereby enhancing overall catalytic efficiency compared to single\u2010site catalysts. This approach effectively decouples complex reaction networks into a sequence of coordinated elementary steps, thereby enhancing the production efficiency of the target products. Here, we propose a relay catalysis paradigm through electrochemical in situ construction of NiOOH\u2010Mo\n                    <jats:sub>2<\/jats:sub>\n                    C@C heterojunction featuring with dual Lewis acid sites. By precisely controlling interfacial methanol\/OH\n                    <jats:sup>\u2212<\/jats:sup>\n                    concentration gradients, nearly 100% Faradaic efficiency for formate production is achieved during methanol electrooxidation. Multiscale characterizations combined with density functional theory computations reveal that the engineered interface regulates *CHO intermediate migration from NiOOH to Mo\n                    <jats:sub>2<\/jats:sub>\n                    C domains, thereby effectively shifting the rate\u2010determining step from *CHO\u2010OH\n                    <jats:sup>\u2212<\/jats:sup>\n                    coupling to O\u2500H bond cleavage. This spatial decoupling strategy reduces the thermodynamic barrier by 1.18\u00a0eV. This study elucidates a design strategy that tailors the spatial distribution of electrochemical interface species to guide catalytic pathway optimization. Furthermore, it highlights the essential role of heterojunction\u2010mediated relay catalysis in enhancing electrocatalytic activity for the oxidation of organic small molecules.\n                  <\/jats:p>","DOI":"10.1002\/anie.202506215","type":"journal-article","created":{"date-parts":[[2025,9,1]],"date-time":"2025-09-01T12:39:32Z","timestamp":1756730372000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":53,"title":["Regulation of Relay Catalytic Mechanism for Efficient Methanol Oxidation Reaction"],"prefix":"10.1002","volume":"64","author":[{"given":"Guangliang","family":"Lin","sequence":"first","affiliation":[{"name":"Frontiers Science Center for New Organic Matter, Key Laboratory of Advanced Energy Materials Chemistry (Ministry of Education), State Key Laboratory of Advanced Chemical Power Sources, Collaborative Innovation Center of Chemical Science and Engineering (Tianjin) College of Chemistry, Nankai University  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300071 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8604-9689","authenticated-orcid":false,"given":"Jun","family":"Chen","sequence":"additional","affiliation":[{"name":"Frontiers Science Center for New Organic Matter, Key Laboratory of Advanced Energy Materials Chemistry (Ministry of Education), State Key Laboratory of Advanced Chemical Power Sources, Collaborative Innovation Center of Chemical Science and Engineering (Tianjin) College of Chemistry, Nankai University  Tianjin 300071 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