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Practical alternative procedures are described for the syntheses of octavinylsilsesquioxane 1, octaphenylsilesquioxane and octabenzylsilsesquioxane. The hydrolytic polycondensation of RSiX3 (R = CH2=CH-, C6H5- or C6H5CH2-; X = Cl, OCH3, or OC2H5) in the presence of solid acid or base Amberlite ion-exchange resin gave improved yields of the corresponding octameric oligosilsesquioxanes. Repetitive usage of the Amberlite resin as the hydrolysis reagent was tested during synthesis of 1. The results indicate that it could be used many times in the same solvent making the procedure a more economically viable technique.

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