TEMPO (2,2,6,6-tetramethylpiperidine-1-oxyl)-mediated oxidation of methyl α-D-glucopyranoside (MGP) was performed in the present of calcium hypochlorite (CaO2Cl2) as co-catalyst, instead of sodium bromide.The primary hydroxyl of MGP was oxidated selectively into corresponding carbonyl compound in this catalytic system.When the oxidation was finished, the metal ions (Ca2+) was removed expediently from the reactive mixture by acidifying in 2M H2SO4 to form calcium sulfate(CaSO4) precipitate isolated easily by filtration.Thus, glucuronic acid was obtained through the hydrolysis of glycosidic bond, and the glucurolactone was synthesized by the esterification in the present of glacicl acetic acid.