Crosslinked resins containing styrylboronic acid units were used in the protection of 1,2 and 1,3‐diol groupings with several acyclic triols. With 1,2,3‐propanetriol, a five‐membered ring boronate was formed almost exclusively while with 1, 2, 4‐butanetriol a six‐membered ring boronate predominated. The fully recyclable polymer could be used in a fast and efficient synthesis of monobenzoyl derivatives of triols. Macroreticular and 1% crosslinked solvent‐swellable resins were tested and the latter were found to perform better on repeated use.
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