1,2,3,4,6-penta-O-acetyl-β-D-glucose is prepared by the reaction of glucose and acetic anhydride.Based on the activity difference and steric hindrance of acetyl in 1,2,3,4,6-pen-ta-O-acetyl-β-D-glucose,4,4’-bis(2,3,4,6-tetra-O-acetyl-β-D-glucoside)-2,2-diphenol propane is prepared by the reaction with1,2,3,4,6-penta-O-acetyl-β-D-glucose and bisphenol-A which structure is symmetric in the presence of dichloromethane.All acetyls of the synthetic products are eliminated in alkali methanol,then a new kind of intermediate of glycophane,4,4’-Bisglucoside-2,2-diphenol propane is obtained.A series of analysis methods including IR analysis、nuclear magnetism resonance(1H NMR)、elementary analysis(EA)and melting point determination are applied to determine products purity and characterize products structure.