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Additionally, the structure\u2010activity relationship of photocatalysts often remains insufficiently explored. Here, a series of thiophene\u2010based covalent triazine frameworks (CTFs) are used for the efficient and selective oxidation of hydrocarbons to aldehydes or ketones under ambient aerobic conditions. Spectroscopic methods conducted in situ and density functional theory (DFT) calculations revealed that the sulfur atoms within the thiophene units play a pivotal role as oxidation sites due to the generation of photogenerated holes. The effect of photogenerated holes on photocatalytic toluene oxidation was investigated by varying the length of the spacer in a CTF donor\u2010acceptor based photocatalyst. Furthermore, the manipulation of reactive oxygen species was employed to enhance selectivity by weakening the peroxidative capacity. As an illustrative example, this study successfully demonstrated the synthesis of a precursor of the neurological drug AMG\u2010579 using a photocatalytic protocol.\n                  <\/jats:p>","DOI":"10.1002\/anie.202400101","type":"journal-article","created":{"date-parts":[[2024,2,26]],"date-time":"2024-02-26T09:40:03Z","timestamp":1708940403000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":46,"title":["Triazine Frameworks for the Photocatalytic Selective Oxidation of Toluene"],"prefix":"10.1002","volume":"63","author":[{"given":"Sizhe","family":"Li","sequence":"first","affiliation":[{"name":"Department of Materials Science Fudan University  200433 Shanghai P. R. 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