The synthesis and X-ray crystal structure of 1,2;5,6-di-O-isopropylidene-3-O-(phenylacetyl)-D-glucofuranose is reported. It crystallizes in the orthorhombic system with space group P212121 (No. 19); a = 9.9313(12) Å, b = 10.0657(12) Å, c = 20.343(2) Å, and Z = 4. The solid state structure is discussed in terms of the use of the title compound for further chemistry.