A series of 1,2-bis(s-triazolo (Bis (S-triazolo[3,4-b][1,3,4]thiadiazolo-3-yl)alkanes 3a–3k were prepared by condensation reaction of 1,2-bis(4-amino-5-mercapto-S-triazol-3-yl)alkanes 1a–1c with N-phetaloyl-l-amino acids 2a–2d in the presence of the phosphoroxy chloride (POCl3) as an anhydrous reagent.