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However, this oxidation process has not yet been achieved in ambient conditions with the aid of oxygen and heterogeneous photocatalysts. In this study, we developed an organic photocatalytic system using covalent triazine\/heptazine\u2010based frameworks (CTF\u2010TB\/CHF\u2010TB) to enable the B\u2013V oxidation reaction under mild conditions through a cascade reaction pathway. Experimental data and theoretical calculations showed that heptazine\/triazine units can \u201cchelate\u201d and decompose the in situ generated H\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    into hydroxyl radicals (\u22c5OH). Compared to conventional methods that primarily involve metal\u2010activated benzaldehyde at elevated temperatures (e.g., 60\u2009\u00b0C), the \u22c5OH generated in our study can readily cleave the C\u2212H bond of benzaldehyde, forming an active intermediate that drives subsequent sequential processes: O\n                    <jats:sub>2<\/jats:sub>\n                    \u2192H\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    \u2192\u22c5OH\u2192Ph\u2010CO\u22c5\u2192Ph\u2010COOO\u22c5. By employing this photocatalytic process, a yield of 91\u2009% and a selectivity of over 99\u2009% were obtained in the oxidation of cyclohexanone to caprolactone at room temperature. This performance is comparable to the state\u2010of\u2010the\u2010art catalysts, and our CHF\u2010TB catalyst demonstrates impressive reusability, maintaining a high yield after 5 consecutive runs. This work presents a straightforward approach for C\u2212H cleavage by organocatalysts to produce\n                    <jats:italic>\u03f5<\/jats:italic>\n                    \u2010caprolactone in a mild manner by B\u2013V oxidation.\n                  <\/jats:p>","DOI":"10.1002\/anie.202416879","type":"journal-article","created":{"date-parts":[[2024,10,18]],"date-time":"2024-10-18T02:10:26Z","timestamp":1729217426000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":45,"title":["Hydroxyl Radical Mediated Heterogeneous Photocatalytic Baeyer\u2013Villiger Oxidation over Covalent Triazine\/Heptazine\u2010Based Frameworks"],"prefix":"10.1002","volume":"64","author":[{"given":"Juntao","family":"Tang","sequence":"first","affiliation":[{"name":"College of Chemistry and Chemical Engineering Central South University  410083 Changsha, Hunan P. R. 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