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As some of the most fundamental and extensively utilized organic chemicals, they play irreplaceable roles across industry, daily life, biological systems, and materials science. Among numerous synthetic approaches to aliphatic carboxylic acids, transition metal\u2010catalyzed direct synthesis from alcohols is particularly compelling, owing to its excellent step economy and environmental sustainability. Therefore, we developed a ruthenium(II)\/diphosphine\u2010catalytic system for the oxidation of primary alcohol with oxygen as terminal oxidant in water, providing a serious of aliphatic carboxylic acids in moderate to excellent efficiencies. Distinct from Ru(II)\u2010catalyzed alcohol acceptorless dehydrogenation reactions that require stoichiometric bases, this transformation may proceed via a single\u2010electron transfer mechanism in the absence of any additives. Furthermore, valence state changes of ruthenium and the diphosphine ligand were observed, with the in situ formed Ru(III)\/Ru(IV) species identified as the actual catalytically active intermediates. The introduction of phosphine ligands increases the electron density of the ruthenium center, thereby facilitating the oxidation of low\u2010valent ruthenium to high\u2010valent ruthenium. This protocol provides an alternative reference for the one\u2010step synthesis of carboxylic acids via low\u2010valent metal\u2010catalytic aerobic oxidation of primary alcohols.<\/jats:p>","DOI":"10.1002\/chem.71246","type":"journal-article","created":{"date-parts":[[2026,6,8]],"date-time":"2026-06-08T12:56:04Z","timestamp":1780923364000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["In Situ Generated Ru(III)\/Ru(IV) From Ru(II) Catalyzed Aerobic Oxidation of Alcohols: Facile Access to Carboxylic Acids in Aqueous Media"],"prefix":"10.1002","volume":"32","author":[{"given":"Lang","family":"He","sequence":"first","affiliation":[{"name":"State Key Laboratory of Low Carbon Catalysis and Carbon Dioxide Utilization Lanzhou Institute of Chemical Physics Chinese Academy of Sciences  Lanzhou PR 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