The periodateoxidation of some derivatives of sucrose at primary positions is generally selective for the D-glucopyranoside group. A cleavage at C-2-C3 or C-3-C-4 positions was observed for the 6,1',6'-tri-O-trityl and 6,1',6'-tri-O-(tert-butyldemethylsilyl) derivatives, respectively. The periodateoxidation was more complete for all other derivatives with a cleavage at C-2-C-3 and C-3-C-4.