The present investigation deals with synthesis & characterization of novel biphenyls containing quinoxaline moiety 2,3-bis (hydroxy phenyl) Quinoxaline 2,3-bis (2-hydroxy naphthalene-6'yl) quinoxaline.The work has been divided into four chapters. The general introduction & type of high performance materials, literature survey in Chapter-I. The measurement & actors affecting the thermal stability, structure, property relationship process ability and their applications in varies fields also discussed in Chapter-II. The synthesis of novel quinoxaline moiety containing bisphenol, 2,3-bis (4-hydroxy phenyl) quinoxaline (IV) & polyesters thereform. A well developed interfacial polycondensation method was used to prepare polyesters with IPC, TPC, or mixure or IPC and TPC in different mole proportional to yield high molecular weight polyester in Chapter-III. Incorporation of bulky PENDANT group into polymer into one of the approaches to improve the solubility without losing applicable thermal stability. Novel 2,3-bis (2-hydroxy naphthalene-6'yl) quinoxaline (IV) was prepared & characterized by spectral methods.