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Herein, a series of azoxy compounds were constructed via facile coupling reactions by using cost\u2010effective <jats:italic>N<\/jats:italic>\u2010methoxyformamide and nitroso compounds over Cu\u2010based catalysts, affording high product yields with excellent tolerance of functional groups. Significantly, the mesoporous silica nanosphere\u2010encapsulated ultrasmall Cu (Cu@MSN) catalyst was developed via a one\u2010pot synthetic method and first used for the synthesis of azoxy compounds. As compared with copper salt catalysts, the Cu@MSN catalyst exhibited remarkably enhanced catalytic activity and superior recycling stability. Such a Cu@MSN catalyst overcame the inherent drawbacks of low activity, fast deactivation, and difficult recycling of traditional metal salt catalysts in organic reactions. This work provides a green and efficient method for the construction of azoxy compounds and also creates new prospects for the application of nanoporous materials confined metal catalysts in organic synthesis.<\/jats:p>","DOI":"10.1002\/cssc.202300477","type":"journal-article","created":{"date-parts":[[2023,5,6]],"date-time":"2023-05-06T06:08:32Z","timestamp":1683353312000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":6,"title":["Synthesis of Azoxy Compounds: from Copper Compounds to Mesoporous Silica\u2010Encaged Ultrasmall Copper Catalysts"],"prefix":"10.1002","volume":"16","author":[{"given":"Zhi\u2010Peng","family":"Han","sequence":"first","affiliation":[{"name":"College of Chemistry Chemical Engineering and Materials Science Soochow University  215123 Suzhou Jiangsu P.\u2005R. 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