A series of a non‐symmetric dimmer of the type 4‐((4‐(((4‐(bromoalkyloxy)benzylidene)amino)methyl)benyl)imino)methyl)phenyl‐4‐(alkyloxy)benzoate contains Br terminal atoms are synthesized and characterized. The molecular structure of these compounds possessed four aromatic rings interconnected via two azomethine linking groups. In each molecule, the two identical methylene spacers vary from either C4H8 or C6H12 are present. The synthesized compounds are characterized using FT‐IR, 1H NMR, and 13C NMR. The results demonstrate the formation of the suggested structures of the prepared structures.