Methyl N-(benzyloxycarbonylaminoacyl)-β-D-glucosaminides and N-(benzyloxycarbonylaminoacyl)-D-glucosaminols were prepared and the periodate oxidation of some of these compounds was studied. Saponification of N-(β-benzyl-N-benzyloxycarbonyl-α-L-aspartyl)-tri-O-acetyl-D-glucosaminide (IIId) caused a transpeptidation to give the β-aspartyl derivative (IVd) and the α-isomer (IVf) was prepared by deacetylation of N-(N-benzyloxycarbonyl-α-aspartyl)-tri-O-acetyl-D-glucosaminide (IIIf), which was obtained by the reaction of N-benzyloxycarbonyl-L-aspartic anhydride with methyl-tri-O-acetyl-β-D-glucosaminide (II).