Fully protected 1-thioglycopyranosyl esters ofN-acylamino acids (5,6, and7) were prepared by condensation of methyl 2, 3, 4-tri-O-acetyl-1-thio-β-d–glucopyranuronate (1), 2, 3, 4-tri-O-acetyl-1-thio-l–arabinopyranose (2), and 2, 3, 4-tri-O-acetyl-1-thio-D-arabinopyranose (3) with pentachlorophenyl esters ofN-acylamino acids in the presence of imidazole. The13C NMR chemical shifts of the starting 1-thio sugars and the 1-thiol ester products are reported.