m-Acetylphenyl-β-d-glucopyranosides and m-acetylphenyl-α/β-d-mannopyranosides were synthesized by the Koenigs–Knorr, Mitsunobu, and Helferich reactions as key glycosylation reactions, respectively. Their spectroscopic properties and antioxidative activities were characterized as potential ultraviolet B-ray absorbents.