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Herein, we report an innovative photoinduced low\u2010valent zirconocene catalysis enabling the reductive coupling of ethers with high activity and cross\u2010selectivity. Mechanistic investigation suggests that photoexcitation of low\u2010valent zirconocene facilitates the C(\n                    <jats:italic>sp3<\/jats:italic>\n                    )\u2212O bond scission of benzylic ethers, leading to the benzylic radicals intermediate via a single\u2010electron reduction pathway. The subsequent recombination of this benzylic radical with the Zr center followed by carbomagnesiation generates benzylic Grignard reagents for downstream coupling with aliphatic ethers through an S\n                    <jats:sub>N<\/jats:sub>\n                    2\u2010like mechanism. In application, a wide range of ethers readily in situ derived from aldehydes and ketones becomes feasible with high functional group compatibility as well as excellent cross\u2010selectivity.\n                  <\/jats:p>","DOI":"10.1002\/anie.202405449","type":"journal-article","created":{"date-parts":[[2024,5,23]],"date-time":"2024-05-23T12:40:15Z","timestamp":1716468015000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":7,"title":["Photoinduced Low\u2010Valent Zirconium Catalysis for Cross\u2010Electrophile Coupling of Ethers"],"prefix":"10.1002","volume":"63","author":[{"given":"Ping","family":"Guo","sequence":"first","affiliation":[{"name":"Key Laboratory for Advanced Materials and Joint International Research Laboratory of Precision Chemistry and Molecular Engineering Feringa Nobel Prize Scientist Joint Research Center Frontiers Science Center for Materiobiology and Dynamic Chemistry School of Chemistry and Molecular Engineering East China University of Science and Technology  Shanghai 200237 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xuedong","family":"Song","sequence":"additional","affiliation":[{"name":"Key Laboratory for Advanced Materials and Joint International Research Laboratory of Precision Chemistry and Molecular Engineering Feringa Nobel Prize Scientist Joint Research Center Frontiers Science Center for Materiobiology and Dynamic Chemistry School of Chemistry and Molecular Engineering East China University of Science and Technology  Shanghai 200237 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Banruo","family":"Huang","sequence":"additional","affiliation":[{"name":"Department of Chemistry University of California  Berkeley California 94720 United States"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ruixue","family":"Zhang","sequence":"additional","affiliation":[{"name":"Key Laboratory for Advanced Materials and Joint International Research Laboratory of Precision Chemistry and Molecular Engineering Feringa Nobel Prize Scientist Joint Research Center Frontiers Science Center for Materiobiology and Dynamic Chemistry School of Chemistry and Molecular Engineering East China University of Science and Technology  Shanghai 200237 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-0451-0919","authenticated-orcid":false,"given":"Jie","family":"Zhao","sequence":"additional","affiliation":[{"name":"Key Laboratory for Advanced Materials and Joint International Research Laboratory of Precision Chemistry and Molecular Engineering Feringa Nobel Prize Scientist Joint Research Center Frontiers Science Center for Materiobiology and Dynamic Chemistry School of Chemistry and Molecular Engineering East China University of Science and Technology  Shanghai 200237 China"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2024,7,9]]},"reference":[{"key":"e_1_2_3_1_1","doi-asserted-by":"publisher","DOI":"10.1002\/9783527813827.ch9"},{"key":"e_1_2_3_2_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.chempr.2023.02.010"},{"key":"e_1_2_3_3_1","first-page":"403","volume-title":"Science of Synthesis: Base-Metal Catalysis 1","author":"Shu X. 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