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However, due to its poor reversibility and excessive random reactive sites, the synthesis of crystalline organic polymers\/frameworks by Friedel\u2010Crafts reaction has never been realized so far. Herein, we develop a molecular confined Friedel\u2010Crafts reaction strategy to achieve rapid preparation (within only 30 minutes) of highly crystalline covalent triazine frameworks (CTFs) with tailorable functionality for the first time. Theoretical calculations and detailed experiments revealed the critical role of carboxyl groups in aromatic benzene monomer during the CTFs crystallization, which can not only effectively cause a suitable activation barrier for the electrophilic attack of 2,4,6\u2010trichloro\u20101,3,5\u2010triazine through their electron\u2010withdrawing properties, but also introduce anchoring effects (molecular confinement effects) to facilitate the ordered polymerization at specific sites in 2D planar direction. Benefiting from the convenient synthetic route and low\u2010cost raw materials, we could unprecedentedly realize the kilogram\u2010scale fabrication of carboxyl\u2010functionalized high\u2010crystalline CTFs. Moreover, thanks to the hydrophilic and ionizable properties of carboxyl groups, the obtained functionalized CTFs exhibited excellent aqueous dispersibility and superior solution processability.<\/jats:p>","DOI":"10.1002\/anie.202421251","type":"journal-article","created":{"date-parts":[[2025,1,13]],"date-time":"2025-01-13T04:12:48Z","timestamp":1736741568000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":13,"title":["Rapid and Scalable Preparation of High\u2010Crystalline Carboxyl\u2010Functionalized Covalent Triazine Frameworks via Friedel\u2010Crafts Reaction"],"prefix":"10.1002","volume":"64","author":[{"given":"Lei","family":"Zhang","sequence":"first","affiliation":[{"name":"School of Engineering Westlake University  Hangzhou 310024, Zhejiang Province China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Tian","family":"Sun","sequence":"additional","affiliation":[{"name":"School of Engineering Westlake University  Hangzhou 310024, Zhejiang Province China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zhao","family":"Zhang","sequence":"additional","affiliation":[{"name":"School of Engineering Westlake University  Hangzhou 310024, Zhejiang Province China"},{"name":"Tianmushan Laboratory  Hangzhou 311115, Zhejiang Province China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ziyue","family":"Zhang","sequence":"additional","affiliation":[{"name":"School of Materials Science and Engineering, Zhejiang Sci-Tech University  Hangzhou 310018, Zhejiang Province China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0318-8515","authenticated-orcid":false,"given":"Yuxi","family":"Xu","sequence":"additional","affiliation":[{"name":"School of Engineering Westlake University  Hangzhou 310024, Zhejiang Province China"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2025,1,21]]},"reference":[{"key":"e_1_2_7_1_1","unstructured":"\u00a0"},{"key":"e_1_2_7_2_2","doi-asserted-by":"publisher","DOI":"10.1021\/ja508693y"},{"key":"e_1_2_7_3_2","doi-asserted-by":"publisher","DOI":"10.1002\/ange.202400101"},{"key":"e_1_2_7_4_2","doi-asserted-by":"publisher","DOI":"10.1038\/s41467-020-19180-3"},{"key":"e_1_2_7_5_1","unstructured":"\u00a0"},{"key":"e_1_2_7_6_2","doi-asserted-by":"publisher","DOI":"10.1021\/jacs.6b07644"},{"key":"e_1_2_7_7_2","doi-asserted-by":"publisher","DOI":"10.1021\/ja304879c"},{"key":"e_1_2_7_8_2","doi-asserted-by":"publisher","DOI":"10.1039\/c3ee42548g"},{"key":"e_1_2_7_9_1","unstructured":"\u00a0"},{"key":"e_1_2_7_10_2","doi-asserted-by":"publisher","DOI":"10.1002\/anie.201511553"},{"key":"e_1_2_7_11_2","author":"Lu X.-M.","year":"2024","journal-title":"Angew. 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