Silica supported sodium hydrogen sulfate (NaHSO₄•SiO₂) has been found to be an efficient heterogeneous catalyst for the reaction of dicarboxylic acids with alcohols (methanol, alcohol, butanol and benzyl alcohol) to give the corresponding dicarboxylic acid esters. This method has high yield and convenient post-treatment, and the catalyst could be easily recovered from the reaction mixture. The crystal of the compound 3k was confirmed by X-ray single-crystal diffraction analysis. The crystal of the compound 3k belongs to Orthorhombic, space group Pbca with cell parameters a＝1.0216(10) nm, b＝0.82794(10) nm, c＝1.7996(2) nm, α＝90°, V＝1.5221(3) nm³, D_c＝1.302 Mg/m³, Z＝4, F(000)＝632, μ＝0.092 mm^－1, R＝0.0518, wR＝0.1475.

Key words: dicarboxylic acid, dicarboxylic acid ester, NaHSO₄•SiO₂, catalysis