Kinetic data of the Zn(Ⅱ) ion-catalyzed hydrolysis of 2-acetylpyridineketoximyl acetate (S) are measured. The reaction proceeds through the accumulation of an intermediate (I). 2-Acetylpyridineketoxime (Ox) is released in the breakdown step of I. Phenol is not formed as a part of the products, and, therefore, diphenyl phosphate and Ox are produced by the breakdown of I. Based on the dependence of the rates for the formation and the breakdown of I on [Zn(Ⅱ)] and pH, and considering the UV spectral properties of I, the structure of I is tentatively assigned as the penta-covalent intermediate formed by the addition of a water molecule to S.