2,5-dibromoterephthalic acid is firstly converted into acryl chloride intermediates by acylation reaction, and further reacts with 4-amino-2,2,6,6-tetramethylpiperidineoxyl (4-NH2-TEMPO) resulting in di-TEMPO function-alized organic building blocks. Sonogashira coupling reaction between the di-TEMPO monomer and tetrakis(4-ethynylphenyl)methane leads to the formation of high density TEMPO radical functionalized conjugated microporous polymers (CMPs), named CMP-4-(TEMPO)2. The chemical composition and structural information of the corresponding monomer and polymers are characterized by NMR, SEM, PXRD, and EPR spectra. CMP-4-(TEMPO)2 consists microspheres and nanotubes, and possesses high BET surface areas (486 m2/g) with micro-, meso- and macropores. The high density of TEMPO radicals in CMP-4-(TEMPO)2 enable highly efficient oxidation of a broad range of alcohols, including aromatic al-cohols, heteroatomic alcohols and fatty alcohols, into their aldehydes and ketones with excellent selectiv-ity.