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However, the C-5 carboxylate of glucuronic acid renders glucuronosyl donors poor electrophiles and glucuronosyl acceptors weak nucleophiles, often leading to unproductive glycosylation. We disclose a robust, general gold(I)-catalyzed \u03b2-glucuronidation using glucuronosyl 8-alkynyl-1-naphthoate donors with the assistance of AgOTf catalysis. Mechanistic studies reveal the role of AgOTf: it promotes orthoester-to-\u03b2-glycoside conversion, likely through trace acid generated from the interaction of Ag+ with adventitious moisture, while HOTf generated in situ from \u2013OTf facilitates regeneration of the active Au(I) catalyst from the resting-state vinyl\u2013digold complex. The method is compatible with diverse substrates and protecting-group patterns, including strongly electron-withdrawing substituents that attenuate the reactivity. Leveraging this platform, we achieve a convergent synthesis of \u03b2-(1 \u2192 4)-polyglucuronate (glucuronan) up to a 32-mer, addressing one of the most demanding linkage patterns in anionic polysaccharide construction.<\/jats:p>","DOI":"10.1021\/jacs.6c10448","type":"journal-article","created":{"date-parts":[[2026,8,4]],"date-time":"2026-08-04T13:13:14Z","timestamp":1785849194000},"page":"33671-33682","source":"Crossref","is-referenced-by-count":6,"title":["AgOTf-Assisted \u03b2-Glucuronidation\nEnables\nConvergent Synthesis of \u03b2-(1 \u2192 4)-Linked Polyglucuronates\nup to the 32-Mer"],"prefix":"10.1021","volume":"148","author":[{"given":"Xinyang","family":"Jiang","sequence":"first","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Zhongshan, China, 528400"]},{"name":"University of Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Can","family":"Jin","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Zhongshan, China, 528400"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Peifan","family":"Xu","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Zhongshan, China, 528400"]},{"name":"Zunyi Medical University , , ,","place":["Zhuhai, China, 519090"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Liran","family":"Yang","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Zhongshan, China, 528400"]},{"name":"Guangzhou University of Chinese Medicine , , ,","place":["Guangzhou, China, 510006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Qing","family":"Wang","sequence":"additional","affiliation":[{"name":"Nanjing University of Chinese Medicine , , ,","place":["Nanjing, China, 210023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xiang","family":"Cao","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Zhongshan, China, 528400"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Wenchao","family":"Zhang","sequence":"additional","affiliation":[{"name":"Nanjing University of Chinese Medicine , , ,","place":["Nanjing, China, 210023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Qing","family":"Han","sequence":"additional","affiliation":[{"name":"Nanjing University of Chinese Medicine , , ,","place":["Nanjing, China, 210023"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0007-8895-7788","authenticated-orcid":true,"given":"Shiyang","family":"Shen","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Zhongshan, China, 528400"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8140-9259","authenticated-orcid":true,"given":"Kan","family":"Ding","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Zhongshan, China, 528400"]},{"name":"University of Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-7864-7045","authenticated-orcid":true,"given":"Yugen","family":"Zhu","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Zhongshan, China, 528400"]},{"name":"University of Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]},{"name":"Guangzhou University of Chinese Medicine , , ,","place":["Guangzhou, China, 510006"]},{"name":"Nanjing University of Chinese Medicine , , ,","place":["Nanjing, China, 210023"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,7,28]]},"reference":[{"key":"2026081210075432500_cit1a","volume-title":"Essentials of Glycobiology","author":"Varki","year":"2022"},{"key":"2026081210075432500_cit1b","doi-asserted-by":"publisher","first-page":"2628","DOI":"10.1016\/j.cell.2024.04.028","article-title":"What comes next in glycobiology","volume":"187","author":"Seeberger","year":"2024","journal-title":"Cell"},{"key":"2026081210075432500_cit2","doi-asserted-by":"publisher","first-page":"11337","DOI":"10.1021\/acs.chemrev.7b00162","article-title":"Chemical Synthesis\nof Oligosaccharides Related to the Cell Walls of Plants and Algae","volume":"117","author":"Kinnaert","year":"2017","journal-title":"Chem. 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