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However, the catalytic stereoselective construction of axially chiral ring scaffolds with more than two axes on a single benzene ring remains a challenging task. Herein, we present an efficient method for synthesizing triaxially chiral polysubstituted naphthalene scaffolds via sequential Ni(II)\u2010catalyzed Diels\u2013Alder reaction of isobenzofurans and TfOH\u2010promoted dehydrative aromatization reaction. Using 1,3\u2010biarylisobenzofurans and \u03b2\u2010aryl\u2010substituted \u03b1,\u03b2\u2010unsaturated\n                    <jats:italic>N<\/jats:italic>\n                    \u2010acyl pyrazoles as modular reaction partners, a series of naphthalenes with 1,3,4\u2010triaxes were synthesized with excellent enantioselectivities and diastereoselectivities. Furthermore, by attaching two pyrene chromophores to this novel triaxially chiral ring scaffold, a circularly polarized luminescence (CPL)\u2010active dye exhibiting a remarkable luminescence dissymmetry factor (\n                    <jats:italic>g<\/jats:italic>\n                    <jats:sub>lum<\/jats:sub>\n                    =\u22120.019) and high fluorescence quantum efficiency (\u00d8\n                    <jats:sub>FL<\/jats:sub>\n                    =0.29) was obtained, highlighting the potential applications of atropisomers with multiple stereogenic axes in the design of chiroptical organic materials.\n                  <\/jats:p>","DOI":"10.1002\/anie.202421060","type":"journal-article","created":{"date-parts":[[2024,12,9]],"date-time":"2024-12-09T08:21:06Z","timestamp":1733732466000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":19,"title":["Enantioselective Synthesis of Atropisomeric Tri\u2010Axis Naphthalenes via Diels\u2013Alder Reaction and Dehydrative Aromatization of Isobenzofurans"],"prefix":"10.1002","volume":"64","author":[{"given":"Yuan\u2010Bo","family":"Du","sequence":"first","affiliation":[{"name":"Department of Chemistry Fudan University  220 Handan Rd. 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