Abstract 1,3,4-Oxadiazoles has been widely used in various fields. The synthesis of symmetrically 2,5-disubstituted 1,3,4-oxadiazoles from diacylhydrazines prepared from acid chloride and hydrazine can be performed by using cyclodehydrating agents. In this paper, 2,5-bis(4-alkoxy-phenyl)-1,3,4-oxadiazoles were synthesized from methy 4-hydroxybenzoate and 4-cyanophenol. The process of experiments was simple, the conditions were mild and the yields were quite good. Hydrogen chloride gases needed in the experiment were prepared from dropping acetylchloride into ethanol which was also the solvent of the reaction. This method can avoid the trouble caused by flowing hydrogen chloride gases directly. The structures were characterized by 1H NMR and 13C NMR.