Arylenedioxy-organosilanylene polymers with adamantane units in the backbone were prepared by Rh-catalyzed dehydrocoupling of bis(4-hydroxyphenyl)adamantanes with organohydrosilanes, and their heat resistance was evaluated by thermogravimetric analysis in nitrogen. Among these polymers, the highest Td10 (10% weight loss temperature) of 547 °C was achieved for polymer 2a prepared from 1,3-bis(4-hydroxyphenyl)adamantane and phenylsilane. Polymer 2a exhibited good heat resistance even in air with Td10 = 387 °C, and standing of the polymer at 150 °C for 8 h resulted in no evident weight loss
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