A novel synthesis of linear high‐molecular‐weight poly(4‐vinylphenol) (PVPh) and poly[styrene‐co‐(4‐vinylphenol)] (STVPh, 2) via demethylation reaction is developed. The parent polymers, poly(4‐methoxystyrene) and poly[styrene‐co‐(4‐methoxystyrene)] produced by free‐radical polymerization, are converted to PVPh and STVPh (2), respectively, by being treated with trimethylsilyl iodide (TMSI) at room temperature. Both 1H NMR and 13C NMR data show that methoxy is completely cleaved and converted to hydroxy after hydrolysis without crosslinking and other side reactions. In addition, size‐exclusion chromatography data show that no chain scission occurs during group conversion.
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Xiang et al. (1995) studied this question.
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