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3,6-di-O-acetyl-4-O-(2,3,4,6-tetra-O-acetyl-(-D-galactopyranosyl)-2-azido-2-deoxy- (-D-glucoppyranosyl nitrate could be separated from its mannose type isomer by glycosylation according to the reactivity difference of these two compounds.The pure glucose type nitrate can be converted to corresponding trichloroacemidate,which reacted with spacer arms in solution of CH2Cl2 with BF3@Et2O as promoters to give desired glycosides and dimers.