In this study, synthesis of symmetric compounds of 2,2′‐(p‐phenylene)bisbenzothiazole, 2,2′‐(p‐phenyl‐ene)bisbenzimidazole and 5,5′‐dimethyl‐2,2′‐(p‐phenylene)bisbenzoxazole were benefited from the reaction of terephthalohydroxamoyl chloride with 2‐amino‐4‐methyl phenol, o‐aminothio phenol and o‐phenylenedi‐amin compounds. The structures of these compounds were confirmed by elemental analysis, mass, 1H‐NMR and FT‐IR techniques.