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Nevertheless, the carbonylative synthesis of alkyl ketones, particularly those incorporating secondary or tertiary alkyl fragments, remains underexplored and poses significant challenges. Herein, we present a nickel\u2010catalyzed carbonylative reductive cross\u2010coupling reaction to synthesize a wide range of aryl\u2010alkyl ketones from readily available alkyl halides, aryl iodides, and Mo(CO)\n                    <jats:sub>6<\/jats:sub>\n                    . This protocol exhibits excellent compatibility with primary, secondary, and tertiary alkyl electrophiles as well as aryl electrophiles bearing electron\u2010withdrawing or electron\u2010donating groups, offering a general access to aryl\u2010alkyl ketones under mild conditions. Mechanistic studies reveal that Mo(CO)\n                    <jats:sub>6<\/jats:sub>\n                    not only serves as a safe and effective CO surrogate, but also plays a crucial role in facilitating the nickel carbonyl species, which is critical for promoting the selective synthesis of aryl\u2010alkyl ketones.\n                  <\/jats:p>","DOI":"10.1002\/asia.202500214","type":"journal-article","created":{"date-parts":[[2025,2,13]],"date-time":"2025-02-13T07:31:31Z","timestamp":1739431891000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["A General Access to Aryl\u2010Alkyl Ketones via Nickel\u2010Catalyzed Carbonylative Reductive Cross\u2010Coupling Reactions"],"prefix":"10.1002","volume":"20","author":[{"given":"Lei","family":"Su","sequence":"first","affiliation":[{"name":"Frontiers Science Center for Transformative Molecules Shanghai Key Laboratory for Molecular Engineering of Chiral Drugs Shanghai Jiao Tong University  Shanghai 200240 China"},{"name":"School of Chemistry and Chemical Engineering Shanghai Jiao Tong University  Shanghai 200240 China"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Shen","family":"Gao","sequence":"additional","affiliation":[{"name":"Frontiers Science Center for Transformative Molecules Shanghai Key Laboratory for Molecular Engineering of Chiral Drugs Shanghai Jiao Tong University  Shanghai 200240 China"},{"name":"School of Chemistry and Chemical Engineering Shanghai Jiao Tong University  Shanghai 200240 China"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Lijuan","family":"Chen","sequence":"additional","affiliation":[{"name":"School of Chemistry and Chemical Engineering Shanghai Jiao Tong University  Shanghai 200240 China"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Jie","family":"Yan","sequence":"additional","affiliation":[{"name":"Henan Energy Chemical Group Co. 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