Two novel kinds of alcohol‐soluble ladderlike poly(silsesquioxane)s containing side‐chain hydroxy groups (OH‐T1 and OH‐T2) were prepared successfully for the first time by hydrolysis of ladderlike poly(silsesquioxane)s with side‐chain ester groups (Ester‐T1 and Ester‐T2), which were synthesized by stepwise coupling polymerization. A variety of characterization methods including FT‐IR, 1H NMR, 13C NMR, 29Si NMR, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), vapor pressure osmometry (VPO), gel permeation chromatography (GPC), and X‐ray diffraction (XRD) were combined to demonstrate that the obtained alcohol‐soluble polymers have ladderlike structures, although some structural defects still existed.
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