A facile synthesis of 4,6-dideoxy-3-O-methyl-D-xylo-hexose (D-chalcose) is described, which involves the preparation of methyl 4,6-dichloro-4,6-dideoxy-3-O-methyl-D-galactopyranoside (2) by a reaction with sulfuryl chloride, and its reduction to the dideoxy sugar by hydrogenation over Raney nickel.