Synthesis and Structure of Sodium Phenylsiloxanolate

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Abstract

Two different synthetic routes for the formation of sodium phenylsiloxanolate (SPS) have been developed: (i) the cleavage of oligo(phenylsilsesquioxane), OPSSO, by NaOH in n-butyl alcohol and (ii) the reaction of phenyltri-n-butoxysilane, PhSi(n-BuO)3, and NaOH in n-butyl alcohol in the presence of water. From both reactions, (i) and (ii), crystalline sym-cis-{(Na+)4[PhSi(O)O-]4}·8n-BuOH (A) was the product isolated and characterized by X-ray diffraction. Reaction of SPS with Me3SiCl resulted in the formation of the corresponding sym-cis-tetraphenyltetrakis(trimethylsiloxy)cyclotetrasiloxane, [PhSi(O)OSiMe3]4. Under anhydrous conditions, PhSi(n-BuO)3 and NaOH reacted to give sodium phenyldi-n-butoxysilanolate, PhSi(ONa)(n-BuO)2. Subsequent treatment with Me3SiCl led to the formation of phenyl(trimethylsiloxy)di-n-butoxysilane, PhSi(n-BuO)2(OSiMe3).

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