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Catalytic C(sp<jats:sup>3<\/jats:sup>)\u2212O cross\u2010coupling of alkyl electrophiles with phenols is an unexplored disconnection strategy to the synthesis of alkyl aryl ethers, with the potential to overcome some of the major limitations of existing methods such as C(sp<jats:sup>2<\/jats:sup>)\u2212O cross\u2010coupling and S<jats:sub>N<\/jats:sub>2 reactions. Reported here is a tandem photoredox and copper catalysis to achieve decarboxylative C(sp<jats:sup>3<\/jats:sup>)\u2212O coupling of alkyl <jats:italic>N<\/jats:italic>\u2010hydroxyphthalimide (NHPI) esters with phenols under mild reaction conditions. This method was used to synthesize a diverse set of alkyl aryl ethers using readily available alkyl carboxylic acids, including many natural products and drug molecules. Complementarity in scope and functional\u2010group tolerance to existing methods was demonstrated.<\/jats:p>","DOI":"10.1002\/anie.201808024","type":"journal-article","created":{"date-parts":[[2018,8,29]],"date-time":"2018-08-29T14:28:14Z","timestamp":1535552894000},"page":"13624-13628","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":126,"title":["Decarboxylative C(sp<sup>3<\/sup>)\u2212O Cross\u2010Coupling"],"prefix":"10.1002","volume":"57","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-4678-7251","authenticated-orcid":false,"given":"Runze","family":"Mao","sequence":"first","affiliation":[{"name":"Laboratory of Inorganic Synthesis and Catalysis Institute of Chemical Sciences and Engineering \u00c9cole Polytechnique F\u00e9d\u00e9rale de Lausanne (EPFL), ISIC-LSCI, BCH 3305  Lausanne 1015 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