Abstract: Compound 2,3,4,6-tetra-O-acetyl-β-Ｄ-glycopyranosyl azide was synthesized and characterized by means of single crystal X-ray diffraction. It crystallized in the monoclinic space group P2₁with crystallographic parameters a=0.759　6(6) nm, b=1.518　4(13) nm, c=1.641　2(14) nm, α=90.00°, β=90.045(1) °, γ= 90.00°, Z=2, V=1.893　0 (3)nm³. In the crystal structure of the title compound, the hexopyranosyl ring adopt a normal ⁴C₁ chair conformation and all the substituents occupy equatorial position and the azide group do not adopt beeline structure but has curve phenomena. 

Key words: glycosyl azide, synthesis, crystal structure