Abstract: With the development of life science and technology, carbohydrates in organic chemistry courses should be paid more attention. But in most of the organic chemistry experiment courses in domestic colleges and universities, the experiments about carbohydrates are usually neglected. "Preparation of surcrose octaacetate" as a comprehensive experiment is designed to make up for this deficiency, including synthesis of sucrose octaacetate, purification through recrystallization process, and characterizations by Fourier transform infrared spectrometer (FI-IR), Proton nuclear magnetic resonance (1H NMR), mass spectrometry (MS) and melting point determination. Through the systematic and complete comprehensive design of the experiment, it not only enables students to master the basic unit operation, but also the analysis of the structure of organic compounds, which is beneficial to train the students' comprehensive experimental ability and scientific literacy.