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The first members of the series of poly‐m‐carboranylenesiloxanes were synthesized by the ferric chloride‐catalyzed condensation of methoxy‐ and chloro‐terminated monomers and generally obtained as insoluble crosslinked gums It has now been discovered that long‐chain, linear polymers can be prepared by simple hydrolytic condensation of m‐B10H10C2(SiMe2OSiMe2Cl)2 and m‐B10H10C2(SiMe2OSiMe2OSiMe2Cl)2 at ice bath temperature, as well as by acid‐catalyzed condensation of the corresponding silanols. In addition, phenyl‐substituted copolymers have been obtained which show outstanding thermo‐oxidative stability at elevated temperature. These linear polymers are soluble waxes and liquids with molecular weights between 16,000 and 30,000; they are potentially useful as high‐temperature liquids and coatings and can be cured at room temperature to form elastomers.

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