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Uncatalyzed thermal condensation of isobutylene with paraformaldehyde in acetic acid-acetic anhydride affords principally 3-methyl-3-butene-l-ol acetate and 3-methylene-l ,5-pentanediol diacetate. The latter is the principal product of a similar condensation of 3-methyl-3-butene-l-ol acetate with paraformaldehyde. The structure of these products was established by standard chemical and physical methods. Accessory products of the condensations which were isolated and characterized included methanol, methyl acetate and isoprene glycol diacetate. Isoprene was obtained on pyrolysis of 3-methyl-3-butene-l-ol acetate.Recent studies of the uncatalyzed thermal condensation of olefins with formaldehyde by Bain,2