The synthesis of the dimers was adapted from the previously reported one and adjusted for the solubility properties and size of the targeted ligands, which had an impact on the purification methods that were viable in this case (Scheme 3). Thus, TIPS-Rod3 36 was desilylated as described (TBAF, THF) and the bis-alkyne Rod-3 was chromatographically isolated to remove the tetrabutylammonium salts. CuAAC ligation of 8 was performed at 60 °C, under microwave irradiation, until complete consumption of Rod3 was observed by TLC (9:1 CH2Cl2:MeOH).