1,3-bis (4-p-nitrophenoxy) benzene were synthesized based on the concept of molecular design. Polyimide based on 1,3-bis (4 - p-nitrophenoxy) benzene and Pyromellitic Dianhydride was prepared by traditional two-step method in DMAC solution，and polyamide was imidized by chemistry and ladder heating-up way. FTIR、DSC、HPLC and NMR were used to characterized the structure and purity of diamine monomer synthesized in this paper. The results showed that the purity of 1,3-bis (4 - p-nitrophenoxy) benzene exceed 99%, ladder heating-up process is in favor of imidization of Polyamide.