A new soluble ladder-like polysilsesquioxane with polar lateral aryl ester group, which has good adhesion properties and could be potential precursors of advanced functional materials such as catalyst carriers, polymeric solid electrolytes and microelectronic packaging materials etc., was successfully synthesized by stepwise coupling polymerization (SCP) method. The monomer used, methyl 4-trichlorosilylpropoxybenzoate, was synthesized by hydrosilylation reaction catalyzed by dicyclopentadienylplatinum(II) dichloride (Cp2PtCl2). The titled polymer was characterized by H-1 NMR, Si-29 NMR, FTIR, X-ray diffraction (XRD) and gel permeation chromatography (GPC). The characterization data demonstrate that the polymer possesses a typical ladder-like structure. (C) 2001 Published by Elsevier Science B.V.