Recently we showed novel sonochemical preparation of carbon spheres (CSs) in solution at room temperature and atmospheric pressure. Furthermore, we could produce CSs from various substituted benzenes. FTIR spectra of CSs are mutually alike. Elementary analysis of CSs from styrene and toluene gave mutually similar results. Therefore, it is thought that reaction mechanism of CS formation is possibly similar. In order to clarify the mechanism of production of CS, we investigated products at the early stage of reactions from styrene and toluene by GC analysis. The results suggest that ultrasonic advanced oxidation of aromatic compounds starts the present CS formation and benzaldehyde is possibly a key material on CSs formation.