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Herein we report the syntheses of highly rigid silicon‐ and tin‐containing cyclic and bicyclic compounds with unsaturated organic backbones. The syntheses proceed via di‐lithiated diethynylbenzene derivatives. The protocols for the known precursor compounds were significantly improved in a two‐step one‐pot reaction with yields up to 45 % by alternating addition of the lithiation reagent and starting...
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