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We prepared a series of triazine conjugated organic polymers to photoactivate C\u2212H into aldehyde\/ketone via O<jats:sub>2<\/jats:sub>\u2192H<jats:sub>2<\/jats:sub>O<jats:sub>2<\/jats:sub>\u2192\u22c5OH\u2192Cl\u22c5\u2192Cl<jats:sub>2<\/jats:sub>\u22c5<jats:sup>\u2212<\/jats:sup>. Experiment results showed Cl<jats:sub>2<\/jats:sub>\u22c5<jats:sup>\u2212<\/jats:sup> could successively activate C(sp<jats:sup>3<\/jats:sup>)\u2212H more effectively than Cl\u22c5 to generate unstable dichlorinated intermediates, increasing the kinetic rate ratio of dichlorination to monochlorination by a factor of 2,000 and thus breaking traditional dichlorination kinetic constraints. These active intermediates were hydrolyzed into aldehydes or ketones easily, when compared with typical stable dichlorinated complexes, avoiding chlorinated by\u2010product generation. Moreover, an integrated two\u2010phase system in an acid solution strengthened the Cl<jats:sub>2<\/jats:sub>\u22c5<jats:sup>\u2212<\/jats:sup> mediated process and inhibited product overoxidation, where the conversion rate of toluene reached 16.94\u2005mmol\/g\/h and the selectivity of benzaldehyde was 99.5\u2009%. This work presents a facile and efficient approach for selective conversion of inert C(sp<jats:sup>3<\/jats:sup>)\u2212H bonds using Cl<jats:sub>2<\/jats:sub>\u22c5<jats:sup>\u2212<\/jats:sup>.<\/jats:p>","DOI":"10.1002\/anie.202304699","type":"journal-article","created":{"date-parts":[[2023,7,6]],"date-time":"2023-07-06T08:04:40Z","timestamp":1688630680000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":38,"title":["Cl<sub>2<\/sub>\u22c5<sup>\u2212<\/sup> Mediates Direct and Selective Conversion of Inert C(sp<sup>3<\/sup>)\u2212H Bonds into Aldehydes\/Ketones"],"prefix":"10.1002","volume":"62","author":[{"given":"Qinhua","family":"Zhang","sequence":"first","affiliation":[{"name":"State Key Laboratory of Heavy Oil Processing, Institute of New Energy, College of Chemical Engineering China University of Petroleum (East China)  Qingdao 266580 P. R. 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