6‐[3‐(1‐Adamantyl)‐4‐methoxyphenyl]‐2‐naphthoic acid (1), a promising new compound for the treatment of disorders of keratinization, has been synthesized in [14C]‐labelled form from barium [14C]‐carbonate via labelled benzene. Benzene‐[U‐14C] was converted to 4‐bromo‐methoxybenzene‐[phenyl‐U‐14C] in six steps. Introduction of the adamantyl ring was carried out using 1‐acetoxyadamantane under acid catalysis. 2‐(1‐Adamantyl)‐4‐bromo‐methoxybenzene‐[phenyl‐U‐14C] (2) was converted to a zincate and coupled with methyl 6‐bromo‐2‐naphthoate using a nickel catalyst. The product of the aryl coupling reaction (3) was then saponified to give 6‐[3‐(1‐adamantyl)‐4‐methoxyphenyl‐[phenyl‐U‐14C]]‐2‐naphthoic acid.