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Herein we report an unprecedented photoelectrocatalytic method for the C\u2212H hexafluoroisopropylation of indoles and tryptophan peptides, utilizing the readily available hexafluoro\u20102\u2010propanol (HFIP) as the fluoroalkylation reagent. In this process, HFIP is converted into hexafluoroisopropyl radicals, enabling fluoroalkylation reactions. This study broadens the potential applications of molecular photoelectrocatalysis, highlighting its capacity to enable transformations that are difficult to accomplish through traditional electrochemical or photochemical approaches.<\/jats:p>","DOI":"10.1002\/anie.202423241","type":"journal-article","created":{"date-parts":[[2025,1,23]],"date-time":"2025-01-23T05:37:07Z","timestamp":1737610627000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":29,"title":["Unlocking HFIP for Fluoroalkylation with Molecular Photoelectrocatalysis"],"prefix":"10.1002","volume":"64","author":[{"given":"Yi\u2010Xian","family":"Zheng","sequence":"first","affiliation":[{"name":"State Key Laboratory of Physical Chemistry of Solid Surfaces, Key Laboratory of Chemical Biology of Fujian Province, and College of Chemistry and Chemical Engineering Xiamen University  Xiamen 361005 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