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We report here a regiodivergent reductive hydroxymethylation of terminal alkynes with aqueous formaldehyde to prepare allylic alcohols enabled by visible light photoredox and cobalt dual catalysis. Using readily available, bulk, and cheap aqueous formaldehyde as a simple C1 source, this method allows for the selective production of both linear and branched allylic alcohols in one\u2010step manner. The excellent regioselectivity of the reaction is effectively controlled by adjusting the electronic and steric properties of the ligands. Moreover, regioselective reductive hydroxymethylation of internal alkynes with aqueous formaldehyde has also been achieved by careful selection of ligands. Mechanistic studies reveal a pathway involving ligand\u2010controlled regioselective oxidative cyclometallation of the alkyne and formaldehyde, followed by a protonolysis process, offering new insights into the catalyst design and reaction mechanism.<\/jats:p>","DOI":"10.1002\/anie.202512923","type":"journal-article","created":{"date-parts":[[2025,9,2]],"date-time":"2025-09-02T11:56:52Z","timestamp":1756814212000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":11,"title":["Regiodivergent Ligand\u2010Controlled Cobalt\u2010Catalyzed Reductive Hydroxymethylation of Alkynes with Aqueous Formaldehyde"],"prefix":"10.1002","volume":"64","author":[{"given":"Ning\u2010Xin","family":"Guo","sequence":"first","affiliation":[{"name":"State Key Laboratory of Low Carbon Catalysis and Carbon Dioxide Utilization Suzhou Research Institute of LICP Lanzhou Institute of Chemical Physics (LICP) Chinese Academy of Sciences  Lanzhou 730000 China"},{"name":"University of Chinese Academy of Sciences  Beijing 100049 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zheng\u2010Yang","family":"Gu","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Low Carbon Catalysis and Carbon Dioxide Utilization Suzhou Research Institute of LICP Lanzhou Institute of Chemical Physics (LICP) Chinese Academy of Sciences  Lanzhou 730000 China"},{"name":"College of Textiles and Clothing Key Laboratory for Advanced Technology in Environmental Protection of Jiangsu Province Yancheng Institute of Technology  Jiangsu 224003 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Meng\u2010Wei","family":"Zhu","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Low Carbon Catalysis and Carbon Dioxide Utilization Suzhou Research Institute of LICP Lanzhou Institute of Chemical Physics (LICP) Chinese Academy of Sciences  Lanzhou 730000 China"},{"name":"University of Chinese Academy of Sciences  Beijing 100049 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chen","family":"Chen","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Low Carbon Catalysis and Carbon Dioxide Utilization Suzhou Research Institute of LICP Lanzhou Institute of Chemical Physics (LICP) Chinese Academy of Sciences  Lanzhou 730000 China"},{"name":"University of Chinese Academy of Sciences  Beijing 100049 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-2262-5488","authenticated-orcid":false,"given":"Ji\u2010Bao","family":"Xia","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Low Carbon Catalysis and Carbon Dioxide Utilization Suzhou Research Institute of LICP Lanzhou Institute of Chemical Physics (LICP) Chinese Academy of Sciences  Lanzhou 730000 China"},{"name":"College of Material Chemistry and Chemical Engineering Key Laboratory of Organosilicon Chemistry and Material Technology Ministry of Education Hangzhou Normal University  Hangzhou 311121 China"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2025,9,2]]},"reference":[{"key":"e_1_2_7_1_1","first-page":"1937","volume":"93","author":"Zoltanski A.","year":"2014","journal-title":"Przem. 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