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Building on the industrial process of dimethyl oxalate (DMO) production from CO and methanol, we report in this work a selective electrochemical pathway to convert DMO to dimethyl tartarate (DMT), a precursor to multiple C\n                    <jats:sub>4<\/jats:sub>\n                    \u2010dicarboxylic acids. On a Cu\n                    <jats:italic>\n                      <jats:sub>\u03b1<\/jats:sub>\n                    <\/jats:italic>\n                    catalyst dominated by Cu(111)\u2010like sites, Faradaic efficiency and partial current density for DMT reach 74.7% and 152\u00a0mA\/cm\n                    <jats:sup>\u2212<\/jats:sup>\n                    <jats:sup>2<\/jats:sup>\n                    , respectively, which significantly outperforms Cu\n                    <jats:italic>\n                      <jats:sub>\u03b2<\/jats:sub>\n                    <\/jats:italic>\n                    dominated with Cu(100)\/(110)\u2010like sites. Facet dependence of the C\u2500C coupling is confirmed via reactivity tests on single\u2010crystal Cu surfaces and CO\u2010poison experiments. In situ Raman spectroscopy reveals that DMO adopts distinct adsorption configurations on different Cu facets\u2014planar on Cu(111) and upright on Cu(100)\/(110)\u2014accounting for the selectivity difference of DMT. Mechanistic studies indicate a surface\u2010mediated nonradical pathway, with the initial electron transfer to adsorbed DMO as the rate\u2010determining step for DMT formation. Our work enables the production of C\n                    <jats:sub>4<\/jats:sub>\n                    \u2010dicarboxylic acids via cascade reactions with CO as the initial feedstock.\n                  <\/jats:p>","DOI":"10.1002\/anie.202525091","type":"journal-article","created":{"date-parts":[[2026,2,4]],"date-time":"2026-02-04T06:28:55Z","timestamp":1770186535000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":1,"title":["Electrocatalytic C\u2500C Coupling of Dimethyl Oxalate to C\n                    <sub>4<\/sub>\n                    Dicarboxylate on Cu"],"prefix":"10.1002","volume":"65","author":[{"given":"Yiwei","family":"Liu","sequence":"first","affiliation":[{"name":"College of Chemistry and Molecular Engineering and Beijing National Laboratory for Molecular Sciences Peking University  Beijing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Linke","family":"Fu","sequence":"additional","affiliation":[{"name":"College of Chemistry and Molecular Engineering and Beijing National Laboratory for Molecular Sciences Peking University  Beijing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zebang","family":"Yin","sequence":"additional","affiliation":[{"name":"College of Chemistry and Molecular Engineering and Beijing National Laboratory for Molecular Sciences Peking University  Beijing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yifei","family":"Xu","sequence":"additional","affiliation":[{"name":"College of Chemistry and Molecular Engineering and Beijing National Laboratory for Molecular Sciences Peking University  Beijing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Bingyuan","family":"Chen","sequence":"additional","affiliation":[{"name":"College of Chemistry and Molecular Engineering and Beijing National Laboratory for Molecular Sciences Peking University  Beijing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xiaoxia","family":"Chang","sequence":"additional","affiliation":[{"name":"College of Chemistry and Molecular Engineering and Beijing National Laboratory for Molecular Sciences Peking University  Beijing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-2303-257X","authenticated-orcid":false,"given":"Bingjun","family":"Xu","sequence":"additional","affiliation":[{"name":"College of Chemistry and Molecular Engineering and Beijing National Laboratory for Molecular Sciences Peking University  Beijing China"},{"name":"Ordos Laboratory  Inner Mongolia 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