Coupling of 1,3,5-trichlorobenzene (I) with n-hexylmagnesium bromide (II) produced the corresponding trihexylbenzene (III) (1-3). The title triiodo derivative was then obtained by iodination of (III) with either bis(trifluoroacetoxy)iodobenzene and iodine in CCl4 (1-3) or N-iodosuccinimide in the presence of trifluoromethanesulfonic acid.