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Silsesquioxane formation competing with the deprotonation of alcohol solvents in the presence of a strong base to form alkoxides is reported for the first time. Evidently, sodium isopropoxide is formed during the synthesis of the sodium salt of a double‐decker octaphenylsilsesquioxane tetrasilanolate in 2‐propanol as the solvent, which leads to the formation of unexpected cis‐ and trans‐di[(3‐chloropropyl)isopropoxysilyl]‐bridged double‐decker octaphenylsilsesquioxanes after in situ coupling with 3‐chloropropyltrichlorosilane. The desired products were characterized by 1H NMR, 13C NMR, and 29Si NMR spectroscopy; ESI‐MS; and single‐crystal X‐ray diffraction.
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Ervithayasuporn et al. (2013) studied this question.
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