A simple synthetic route for the efficient preparation and purification of two regioisomers of a pyrene derivative containing two ethynyl groups-1,6- and 1,8-bis(ethynyl)pyrene-is described. The former compound was used as a building block for the stepwise synthesis of a highly conjugated, ditopic bis(2,2'-bipyridine) ligand (2) containing the pyrene nucleus at the central core. The fluorescence properties of ligand 2 are reported. ((c) Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2005).