Butane-1,2,3,4-tetracarboxylic acid is reacted with hydrolyzed 3-aminopropyltriethoxysilane (APTES) at 110 and 220 degrees C (molar ratios 1 : 1 and 1 : 2). The as-prepared materials were characterized by means of various analytical methods. FTIR measurements revealed the formation of a polyamic acid at 110 degrees C whereas the treatment at 220 degrees C resulted in the preparation of a polyimide. These findings were confirmed by means of SS-13C-MAS-NMR. XRPD experiments gave clear evidence for the formation of a specific periodic arrangement in the material. Thermogravimetric analysis indicated that the organicinorganic material has improved thermal properties. All the materials obtained were insoluble in water and organic solvents. (c) 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012