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In particular, the trifluoromethyl ketone group is of great interest due to its role as a carboxylic acid bioisostere. Recently, these fragments have been accessed via acyl radical equivalents. Herein, we disclose an unconventional intramolecular proton\u2010coupled electron transfer activation of \u03b1\u2010keto acids by photoredox catalysis to generate ketyl radicals toward accessing functionalizable lactones. These lactones serve as synthons for modular one\u2010pot syntheses of trifluoromethyl ketones in a net dicarbofunctionalization of electron\u2010rich olefins.<\/jats:p>","DOI":"10.1002\/chem.202501613","type":"journal-article","created":{"date-parts":[[2025,5,22]],"date-time":"2025-05-22T09:31:04Z","timestamp":1747906264000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":3,"title":["Intramolecular PCET of \u03b1\u2010Keto Acids: Synthesis of Trifluoromethyl Ketones via Ketyl Radicals"],"prefix":"10.1002","volume":"31","author":[{"ORCID":"https:\/\/orcid.org\/0000-0001-8261-0838","authenticated-orcid":false,"given":"Rifat N.","family":"Nabi","sequence":"first","affiliation":[{"name":"Department of Chemistry Temple University  1901 North 13th Street Philadelphia Pennsylvania 19122 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0006-1228-7901","authenticated-orcid":false,"given":"Kimberly A.","family":"Jarquin","sequence":"additional","affiliation":[{"name":"Department of Chemistry Temple University  1901 North 13th Street Philadelphia Pennsylvania 19122 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4895-7015","authenticated-orcid":false,"given":"Anupam","family":"Karmakar","sequence":"additional","affiliation":[{"name":"Department of Chemistry Temple University  1901 North 13th Street Philadelphia Pennsylvania 19122 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0007-2417-539X","authenticated-orcid":false,"given":"Kyle E.","family":"Brunner","sequence":"additional","affiliation":[{"name":"Department of Chemistry Temple University  1901 North 13th Street Philadelphia Pennsylvania 19122 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-0667-6170","authenticated-orcid":false,"given":"Daniel K.","family":"Kim","sequence":"additional","affiliation":[{"name":"Department of Chemistry Temple University  1901 North 13th Street Philadelphia Pennsylvania 19122 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2025,5,30]]},"reference":[{"key":"e_1_2_5_1_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.jmedchem.5b00258"},{"key":"e_1_2_5_2_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.jmedchem.7b01788"},{"key":"e_1_2_5_3_1","doi-asserted-by":"publisher","DOI":"10.1002\/cmdc.201200585"},{"key":"e_1_2_5_4_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.bmcl.2023.129363"},{"key":"e_1_2_5_5_1","doi-asserted-by":"publisher","DOI":"10.1039\/c3cc46266h"},{"key":"e_1_2_5_6_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202109235"},{"key":"e_1_2_5_7_1","doi-asserted-by":"publisher","DOI":"10.1021\/jacs.3c04294"},{"key":"e_1_2_5_8_1","doi-asserted-by":"publisher","DOI":"10.1055\/s-0037-1610329"},{"key":"e_1_2_5_9_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.chemrev.8b00782"},{"key":"e_1_2_5_10_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.201501908"},{"key":"e_1_2_5_11_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.201308614"},{"key":"e_1_2_5_12_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.orglett.6b00895"},{"key":"e_1_2_5_13_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.orglett.7b00022"},{"key":"e_1_2_5_14_1","doi-asserted-by":"publisher","DOI":"10.1021\/ja00528a029"},{"key":"e_1_2_5_15_1","doi-asserted-by":"publisher","DOI":"10.1021\/cr400685r"},{"key":"e_1_2_5_16_1","doi-asserted-by":"publisher","DOI":"10.1126\/science.aau1777"},{"key":"e_1_2_5_16_2","doi-asserted-by":"publisher","DOI":"10.1002\/anie.201607176"},{"key":"e_1_2_5_17_1","doi-asserted-by":"publisher","DOI":"10.1126\/science.adp5777"},{"key":"e_1_2_5_18_1","doi-asserted-by":"publisher","DOI":"10.1021\/jacs.3c06347"},{"key":"e_1_2_5_19_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41557-023-01135-y"},{"key":"e_1_2_5_20_1","doi-asserted-by":"publisher","DOI":"10.1021\/jacs.4c10093"},{"key":"e_1_2_5_21_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41467-021-24144-2"},{"key":"e_1_2_5_22_1","doi-asserted-by":"publisher","DOI":"10.1021\/acscatal.2c03996"},{"key":"e_1_2_5_23_1","doi-asserted-by":"publisher","DOI":"10.1039\/D0CS00358A"},{"key":"e_1_2_5_24_1","doi-asserted-by":"publisher","DOI":"10.1021\/ja404342j"},{"key":"e_1_2_5_25_1","doi-asserted-by":"publisher","DOI":"10.3390\/ijms22052769"},{"key":"e_1_2_5_26_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.tetlet.2012.12.003"},{"key":"e_1_2_5_27_1","doi-asserted-by":"publisher","DOI":"10.1021\/jacs.5c00835"},{"key":"e_1_2_5_28_1","volume":"64","author":"Zhang F.","year":"2025","journal-title":"Angew. 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