The efficient method we have developed for the synthesis of some novel biologically active 1,2,4-Triazole Analogues, In case several five-membered aromatic systems having three hetero atoms at the symmetrical position have been studied because of their interesting physiological properties and have broad scope towards the organic transformation. It is also well established that various derivatives of 1,2,4-triazole. This is a convenient method that proceeded under clean, non-toxic, efficient, and mild reaction conditions for synthesizing the first step as a one-pot N-substituted thioureas derivatives in acetonitrile (CH₃CN). In the mechanistic pathway, benzoyl isothiocyanate is formed by the reaction of 3,5-dichlorobenzoyl chloride or 3,5-Bis (Trifluoromethyl) benzoyl chloride with ammonium thiocyanate (NH₄SCN). Afterward, the benzoyl isothiocyanate reacts with aminophenols like (4-Nitro, 4-chloro, 5-Chloro, 4-methyl, and 5-Methyl) to afford the N-Aryl- N’- benzoylthioureas in high yield. To the best of our knowledge, this report describes for the convenient time a procedure focused specifically on the introduction of 1,2,4, triazoles analogs from corresponding N-aryl-N’- benzoylthioureas derivatives using hydrazine hydrate in 1,4- dioxane at 70 °C for 0.5 h to showing good reactivity with electron-donating and electron-withdrawing five-membered heterocyclic examples such as 4-chloro-phenol, 5-chloro phenol, 4-nitrophenol, 4-methylphenol, 3,5-bis(trifluoromethyl)phenyl 4-chlorophenol, 3,5-bis(trifluoromethyl)phenyl 5-chlorophenol 1,2,4,-triazole derivatives, to afford moderate to the high amount of yields.