Abstract Condensation of dimeric 3, 4, 6-tri-O-acetyl-2-deoxy-2-nitroso-α-d-glucopyranosyl chloride with 4-methylumbelliferone gave crystalline 4-methylumbelliferyl 3, 4, 6-tri-O-acetyl- 2-deoxy-2-oximino-α-d-arabino-hexopyranoside. Acetylation of this adduct, reduction of the resulting crude O-acetyloxime with borane in oxolane, and acetylation gave the 3, 4, 6-tri-O- acetyl derivative of 4-methylumbelliferyl 2-acetamido-2-deoxy-α-d-glucopyranoside (1). A ...