The preparation of several bis(1,4‐diazepinium) salts from the reaction of three 1,2‐diamines with a bis(vinamidinium) salt is described. Bis(γ‐substituted pentamethine cyanine(dyes are also prepared from the reaction of vinamidinium salt with 1,2‐dimethylquinolinium perchlorate and 1,2,3,3‐tetramethyl‐3H‐indolium perchlorate. Data from elemental analyzes, IR, 1H‐NMR, 13C‐NMR, and mass spectra (MS) confirm the molecular structure of the obtained products.