Abstract: Octamethoxy-o-quaterphenyl (8a) was prepared in three steps from 4-bromo-1, 2- dimethoxybenzene (5a) employing two base-mediated biaryl couplings. Demethylation of 8a followed by alkylation with decyl bromide gave the tetradecyloxy-o-quaterphenyl (8c). Key words: biaryl coupling, o-quaterphenyl, alkyllithiums