Novel N-(5-aryl-1,3,4-thiadiazol-2-yl)-2-(3-oxo-1,2-benzothiazol-2(3 H)-yl)acetamide derivatives were prepared by 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and N-hydroxybenzotrizole condensation catalysis in a convenient and fast method. These compounds were identified by IR, 1H NMR and elemental analyses and the intermediate compound 5-(2-chlorophenyl)-1,3,4-thiadiazol-2-amine was confirmed by single-crystal X-ray diffraction.