Anisaldehyde was prepared by the ozonolysis of anethole. By experiment, a single solvent system with carbonyl group was fond in which anisaldehyde had a good yield. Meanwhile, the species and mass of solvent and flow of ozone and time of the reactivity were investigated. The optimum conditions are as follows: acetic ether or acetone as solvent, the mass ratio of anethole and solvent is 1:3, the flow of ozone is 0.06 m3/h, the time of the reactivity is 80min. In this condition, the percent conversion of anethole is 100% and the yield of anisaldehyde is 74.54% in ethyl acetate and 73.61% in acetone.