AbstractA synthesis of meta‐terphenyl‐2,4,6,2′,5′,2″,4″,6″‐D8has been carried out. From iodobenzene‐2,4,6‐D3and 2,6‐dibromo‐1,4‐dinitrobenzene, the compound 2′,5′‐dinitro‐meta‐terphenyl‐2,4,6,2″,4″,6″‐D6is formed (Ullmann reaction). By reduction of the nitrogroups and subsequent reductive diazotization, two deuterium atoms are introduced into the centre ring at positions 2′ and 5′. The labelled meta‐terphenyl has been obtained in 15 % yield, based on labelled iodobenzene. Deuterium substitution is ≥ 98% at positions 2,4,6