A series of bis (4-amino-4H-1, 2, 4-triazole-3-thiols) 3a–e were prepared by condensation reactions of 2, 2′-(phenylmethylene) bis (sulfanediyl) diacetic acids 2a–e with thiocarbohydrazide. The starting diacid 2a–e was prepared by reactions of aromatic aldehydes 1a–e with 2-mercaptoacetic acid. The structures of these newly synthesized compounds are characterized by elemental analysis, and infrared and NMR spectroscopy.