The two poly(silyl ester)s containing 2,2bis(p-dimethylsiloxy-phenyl)propane units in the polymer backbones have been prepared via polycondensation reaction of di-tert-butyl adipate and di-tert-butyl fumarate with 2,2-bis(p-chloro dimethylsiloxy-phenyl)propane to give tertbutyl chloride as the condensate. The polymerizations were performed under nitrogen at 110 degrees C for 24 h without addition of solvents and catalysts to obtain the poly(silyl ester)s with weight average molecular weights typically ranging from 5000 to 10,000 g/mol. Characterization of the poly(silyl ester)s included H-1 NMR and C-13 NMR spectroscopies, infrared spectroscopy, ultraviolet spectroscopy, differential scanning calorimetry, thermogravimetric analysis (TGA), gel permeation chromatography, and Ubbelohde viscometer. The glass transition temperatures (T-g) of the obtained polymers were above zero because of the introducing 2,2bis(p-dimethylsiloxy-phenyl)propane units in the polymer backbones. The TGA/DTG results showed that the obtained poly(silyl ester)s were stable up to 180 degrees C and the residual weight percent at 800 degrees C were 18 and 9%, respectively. (c) 2006 Wiley Periodicals, Inc.