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The synthesis of spiroglycol by one-pot reaction was studied using pentaerythritol, isobutyraldehyde and formaldehyde as starting materials. Under the optimum reacting conditions, the yield and purity of product were 93.6 % and 99.0 %, respectively. Compared to the synthesis methods reported in literatures, not only was the yield of product improved, but also two operating units were omitted. The product was characterized by ¹H NMR and IR.