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However, conventional GA synthesis methods suffer from harsh reaction conditions, low selectivity, and high purification costs. Herein, we for the first time demonstrate a new photoredox\u2010catalyzed high\u2010performance route toward dehydrogenative C\u2500C coupling of methanol into GA paired with H\n                    <jats:sub>2<\/jats:sub>\n                    generation over Ni\u2010decorated ZnIn\n                    <jats:sub>2<\/jats:sub>\n                    S\n                    <jats:sub>4<\/jats:sub>\n                    , presenting an essentially untapped photocatalytic tactic for selective GA synthesis. Specifically, GA is formed with the production rate of 30.0 mmol\u00b7g\n                    <jats:sup>\u22121<\/jats:sup>\n                    \u00b7h\n                    <jats:sup>\u22121<\/jats:sup>\n                    and the selectivity of 94% and the optimal apparent quantum yield at \u03bb = 360\u00a0nm reaches 22%, the highest value reported to date for selective photocatalytic methanol conversion to GA. Mechanistic studies reveal that the decoration of Ni facilitates interfacial charge separation and transfer and promotes the formation of key radical intermediates of \u2022CH\n                    <jats:sub>2<\/jats:sub>\n                    OH and \u2022OCH\n                    <jats:sub>3<\/jats:sub>\n                    for GA production. This work offers a conceptually new photocatalytic approach for the efficient and sustainable production of GA and enriches the content of methanol upcycling chemistry.\n                  <\/jats:p>","DOI":"10.1002\/anie.202513406","type":"journal-article","created":{"date-parts":[[2025,10,10]],"date-time":"2025-10-10T08:11:17Z","timestamp":1760083877000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":30,"title":["Methanol Upcycling Toward Glycolaldehyde Synthesis Enabled by New High\u2010Performance Photoredox Route"],"prefix":"10.1002","volume":"64","author":[{"given":"Yu\u2010Fan","family":"Chen","sequence":"first","affiliation":[{"name":"College of Chemistry State Key Laboratory of Photocatalysis on Energy and Environment Fuzhou University  Fuzhou 350116 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ming\u2010Yu","family":"Qi","sequence":"additional","affiliation":[{"name":"School of Materials and Energy &amp; Institute of Fundamental and Frontier Sciences University of Electronic Science and Technology of China  Chengdu 611731 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chang\u2010Long","family":"Tan","sequence":"additional","affiliation":[{"name":"School of Materials and Energy &amp; Institute of Fundamental and Frontier Sciences University of Electronic Science and Technology of China  Chengdu 611731 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zi\u2010Rong","family":"Tang","sequence":"additional","affiliation":[{"name":"College of Chemistry State Key Laboratory of Photocatalysis on Energy and Environment Fuzhou University  Fuzhou 350116 China"},{"name":"School of Materials and Energy &amp; Institute of Fundamental and Frontier Sciences University of Electronic Science and Technology of China  Chengdu 611731 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-2195-1695","authenticated-orcid":false,"given":"Yi\u2010Jun","family":"Xu","sequence":"additional","affiliation":[{"name":"College of Chemistry State Key Laboratory of Photocatalysis on Energy and Environment Fuzhou University  Fuzhou 350116 China"},{"name":"School of Materials and Energy &amp; 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