The synthetic parameters were changed to explore the formation mechanism of the oxygen-containing groups on the surfaces of the hypercrosslinked polymers. The FT-IR spectra and the Boehm titration were used to characterize the surface chemistry of the synthesized polymers. The GC-MS was applied to analyze nitrobenzene which was the solvent in the reaction. The functionalities such as carbonyls and phenols were formed through the oxidation of residual chloromethyl groups by nitrobenzene and the carboxylic groups were formed through further oxidation by oxygen. The nitrobenzene was deoxidized to nitrosobenzene and further to aniline. The Synthetic parameters were changed to explore the formation mechanism of the oxygen-containing groups on the surfaces of the hypercrosslinked polymers. The FT-IR spectra and the Boehm titration were used to characterize the surface chemistry of the synthesized polymers. The GC-MS was applied to analyze nitrobenzene which was the solvent in the reaction. The nitrification of such carbonyls and phenols were formed through the oxidation of residual chloromethyl groups by nitrobenzene and the carboxylic groups were formed through further oxidation by oxygen. The nitrobenzene was deoxidized to nitrosobenzene and further to aniline.