A solution of the diazonium compound obtained from 3, 4-methylenedioxyaniline was decomposed by adding it dropwise into the hot aqueous solution of urea, copper sulfate, and sulfuric acid, the mixture was distilled by the passage of steam, and the distillate was extracted with ether from which sesamol (3, 4-methylenedioxyphenol) was obtained in 12% yield.