The development of an efficient and highly productive synthetic protocol for preparation of new 2,5-diamino-1,3,4-thiadiazole derivatives functionalized with N-(2,2,2-trichloroethyl)carboxamide group was reported.The method of their preparation was based on the reaction of oxidative dehydrosulfurization of N-(2,2,2-trichloro-1-(2-(phenylcarbamothioyl)hydrazine-1-carbothioamido)ethyl)carboxamides and N-(1-(2-carbamothioylhydrazine-1-carbothioamido)-2,2,2-trichloroethyl)benzamide under the action of a mixture of iodine and triethylamine in DMF.This reaction took place at room temperature for two hours and allowed obtaining the target products with a 69-75% yield.Using the developed protocol, ten new derivatives of 1,3,4-thiadiazole were obtained.Their structure was proven by IR,1H NMR,13C NMR, 1H-1H COSY, 1H-13C HSQC, 1H-13C HMBC spectroscopy and LC/HRMS spectrometry.