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However, the synthesis of silacycles\u2500particularly medium-sized rings\u2500remains a formidable challenge. Herein, we report a general and efficient method for accessing a new family of nine- to eleven-membered benzodisilacycles bearing an additional heteroatom (O, S, N, or Si) on the ring scaffolds via palladium-catalyzed intermolecular silylation of primary and secondary C(sp3)\u2013H bonds. Readily available ortho-ether, thioether, tertiary amine, and silyl-substituted aryl iodides, as well as cyclic disilanes, serve as the building blocks, laying the foundation for diversity-oriented synthesis of these novel silacyclic scaffolds (&amp;gt;100 examples). Other salient features include excellent chemoselectivities, broad functional group tolerance, simple reaction conditions, low catalyst loading, and scalability. The key to the high efficiency of this disilylation reaction lies in the employment of cyclic disilanes as the silylation reagents. The synthetic practicality of the current strategy is further proven by the late-stage modification of pharmaceuticals and bioactive compounds.<\/jats:p>","DOI":"10.1021\/jacsau.6c00655","type":"journal-article","created":{"date-parts":[[2026,6,26]],"date-time":"2026-06-26T02:51:07Z","timestamp":1782442267000},"page":"4166-4175","source":"Crossref","is-referenced-by-count":0,"title":["Construction of Medium-Sized\nBenzodisilacycles via\nPalladium-Catalyzed Intermolecular C(sp3)\u2013H Silylation"],"prefix":"10.1021","volume":"6","author":[{"given":"Yingying","family":"Zhang","sequence":"first","affiliation":[{"name":"Zhengzhou University , , ,","place":["Zhengzhou, China, 450001"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Feifan","family":"Gao","sequence":"additional","affiliation":[{"name":"Zhengzhou University , , ,","place":["Zhengzhou, China, 450001"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chong","family":"Li","sequence":"additional","affiliation":[{"name":"Zhengzhou University , , ,","place":["Zhengzhou, China, 450001"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-0134-0870","authenticated-orcid":true,"given":"Yangjie","family":"Wu","sequence":"additional","affiliation":[{"name":"Zhengzhou University , , ,","place":["Zhengzhou, China, 450001"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0000-6477-3529","authenticated-orcid":true,"given":"Ze-Shui","family":"Liu","sequence":"additional","affiliation":[{"name":"Zhengzhou University , , ,","place":["Zhengzhou, China, 450001"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,6,25]]},"reference":[{"key":"2026072709073608800_cit1","doi-asserted-by":"publisher","first-page":"11321","DOI":"10.1002\/anie.201305496","article-title":"Chiral Silanediols\nin Anion-Binding Catalysis","volume":"52","author":"Schafer","year":"2013","journal-title":"Angew. 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