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Although the metal\/oxide interface is highly active and selective, the interfacial sites fall far behind the demand, due to the large and thick support. Herein, we successfully develop a unique Au\u2212CuO Janus structure (average particle size=3.8\u2005nm) with an ultrathin CuO layer (0.5\u2005nm thickness) via a bimetal in situ activation and separation strategy. The resulting Au\u2212CuO interfacial sites prominently enhance isopropanol adsorption and decrease the energy barrier of \u03b2\u2010C\u2212H bond scission from 1.44 to 0.01\u2005eV due to the strong affinity between the O atom of CuO and the H atom of isopropanol, compared with Au sites alone, thereby achieving ultrahigh acetone selectivity (99.3\u2009%) over 1.1\u2005wt\u2009% AuCu<jats:sub>0.75<\/jats:sub>\/Al<jats:sub>2<\/jats:sub>O<jats:sub>3<\/jats:sub>at 100\u2009\u00b0C and atmospheric pressure with 97.5\u2009% isopropanol conversion. Furthermore, Au\u2212CuO Janus structures supported on SiO<jats:sub>2<\/jats:sub>, TiO<jats:sub>2<\/jats:sub>or CeO<jats:sub>2<\/jats:sub>exhibit remarkable catalytic performance, and great promotion in activity and acetone selectivity is achieved as well for other reducible oxides derived from Fe, Co, Ni and Mn. This study should help to develop strategies for maximized interfacial site construction and structure optimization for efficient \u03b2\u2010C\u2212H bond activation.<\/jats:p>","DOI":"10.1002\/anie.202203827","type":"journal-article","created":{"date-parts":[[2022,4,14]],"date-time":"2022-04-14T05:45:30Z","timestamp":1649915130000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":68,"title":["Synergy in Au\u2212CuO Janus Structure for Catalytic Isopropanol Oxidative Dehydrogenation to Acetone"],"prefix":"10.1002","volume":"61","author":[{"given":"Meng","family":"Guo","sequence":"first","affiliation":[{"name":"Key Laboratory of Beijing on Regional Air Pollution Control Beijing Key Laboratory for Green Catalysis and Separation Center of Excellence for Environmental Safety and Biological Effects Beijing University of Technology Beijing 100124 P. R. 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