This work describes the highly efficient acetylation (acylation) of alcohols with acetic acid for the ester synthesis in the presence of newly designed a new composite zirconium (IV) chloride and magnesium catalyst which is used bimetallic acidic catalyst ZrCl 4 -Mg(ClO 4 ) 2 , which is formed by grinding ZrCl 4 and Mg(ClO 4 ) 2 in the molar ratio of 1:2, respectively. Thus, the powder X-ray diffraction, scanning electron microscopy, Brunauer-Emmett-Teller surface area, and thermogravimetric analysis of the ZrCl 4 , Mg(ClO 4 ) 2 , and non-calcined ZrCl 4 -Mg (ClO 4 ) 2 were recorded. In each case, structural analysis was carried by grinding the catalyst in mortar and pestle. K E Y W O R D S acylation, bimetallic acidic catalyst, scanning electron microscopy (SEM), substituted alcohol, ZrCl 4 -Mg(ClO 4 ) 2