ABSTRACTIn-situ filling through hydrolysis and condensation of silicon alkoxides dissolved into polymers has been utilized to generate nanocomposites in which the filler phase can be intimately associated with the polymer on relatively small length scales. One problem of the method has been achieving useful fill volumes without bulk phase separation of the growing inorganic component from the polymer. In this paper, we describe the preparation of a new class of nanocomposite materials in which the inorganic filler phase is pre-assembled before copolymerization with an organic monomer. Maleimide monomers, prepared from alkoxysilylpropyl amines and maleic anhydride, were protected against side reactions by forming the oxonorbornene Diels-Alder adduct with furan. The monomers were then reacted under solgel conditions to form oligomers or polymers making up the filler phase. The material was activated by thermal deprotection of the maleimide and reacted with organic monomers or polymers to form the filled nanocomposite.