Nanostructured titanium oxide difluoride embedded in a matrix of amorphous carbon was synthesized by pyrolysis of D-fructose in the presence of titanium tetrafluoride (optimal Ti/fructose molar ratio = 5.5), both in the solid state at ca. 150 °C and in suspension of 1,2-dichloroethane at reflux temperature. The resulting solid materials were characterized by powder X-ray diffraction (PXRD), transmission electron microscopy (TEM), and elemental analysis. In every case, PXRD and TEM data indicated the presence of an unique crystalline phase (TiOF2) embedded in a light matrix (amorphous carbon). The average crystal size of the powder can be regulated by varying the reaction time.