The one-pot polycondensation of dihydroxyaromatic compounds such as hydroquinone, 2,2-di(4-hydroxy phenyl) propane (Bisphenol A), 4,4'-dihydroxybiphenyl, dihydroxynaphthalenes (1,5- and 2,6-) with 2,5-dimethoxytetrahydrofuran as a reactive protected 1,4-dicarbonyl compound using trifluoroacetic acid as both solvent and condensing agent leads to condensation polymers having linear and ladder structure with high thermal stability. Optimal conditions for polycondensation were obtained via study of the model compounds. All polymers were obtained in high yields and with varying molecular weights (eta = 0.16-0.31 dl/g). The structure of the polymers were characterized by NMR, FTIR spectroscopies and TG. (C) 2010 Elsevier Ltd. All rights reserved.