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However, their structural diversity has long been confined to fully substituted scaffolds due to the stringent requirement for kinetic stabilization and limited synthetic methods, which hampers the exploration of their chemical space. Herein, we report an efficient synthetic route to a variety of less-substituted borirenes, enabled by a crystalline arylchlorohydroborane reagent featuring dual B\u2013H and B\u2013Cl functionalities (aryl = 2,6-(CF3)2phenyl, XylF). The protocol comprises a selective 1,1-hydroboration of alkynes, followed by cooperative NHC- and base-promoted ring-closure. The enhanced \u201cpush\u2013pull\u201d effect induced by the \u03c0-donating group on carbon and the electron-withdrawing XylF group on boron stabilizes these less-sterically protected aromatic borirenes, facilitating their isolation and structural characterization. Consequently, these borirenes readily undergo ring expansion into five- and six-membered boracycles via multiple isocyanide insertions into the polar C\u2013B \u03c3 bond.<\/jats:p>","DOI":"10.1021\/jacs.6c11149","type":"journal-article","created":{"date-parts":[[2026,8,7]],"date-time":"2026-08-07T16:02:11Z","timestamp":1786118531000},"page":"34949-34957","source":"Crossref","is-referenced-by-count":0,"title":["Synthesis\nof Less-Substituted Borirenes Enabled by\na Crystalline Arylhalohydroborane Reagent"],"prefix":"10.1021","volume":"148","author":[{"given":"Chuanbiao","family":"Du","sequence":"first","affiliation":[{"name":"Shanghai Jiao Tong University , , ,","place":["Shanghai, P. R. China, 200240"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zipeng","family":"Zhang","sequence":"additional","affiliation":[{"name":"Shanghai Jiao Tong University , , ,","place":["Shanghai, P. R. China, 200240"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6709-3673","authenticated-orcid":true,"given":"Constantin G.","family":"Daniliuc","sequence":"additional","affiliation":[{"name":"Universita\u0308t Mu\u0308nster , , ,","place":["Mu\u0308nster, Germany, 48149"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-2761-3766","authenticated-orcid":true,"given":"Chaohuang","family":"Chen","sequence":"additional","affiliation":[{"name":"Shanghai Jiao Tong University , , ,","place":["Shanghai, P. R. China, 200240"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,8,7]]},"reference":[{"key":"2026081910250049700_cit1","doi-asserted-by":"publisher","first-page":"585","DOI":"10.1038\/s41557-022-00961-w","article-title":"Aromaticity\nRules","volume":"14","author":"Sola\u0300","year":"2022","journal-title":"Nat. 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