Abstract: Diethyl 2,3-dicyano-2, 3-diphenylsuccinate (I) was synthesized by oxidative coupling" reaction of ethyl a-cyanophenylacetate with Cu⁺⁺-TMEDA-O₂ system. The structure of Iis determined on the basis of IR, ¹HNMR, UV, MSand elemental analysis, and through alkaline hydrolysis of Ito 2,3-diphenylsuccinonitrite. The configuration of Iis identified to be the meso-isomer by x-ray crystallographic analysis in collaboration with the Institute of Physical Chemistry of Beijing University. The conversion-time curves are determined when Iwas used as initiator in the bulk polymerization of styrene at 80, 90,100, 110 and 120℃ respectively. M_w, M_n and dispersion coefficients of polymers obtained with a fixed amount of Ias initiator in the bulk polymerization of styrene at 70, 80, 90, 100, 110, 120 and 150℃ or with various amounts of Ias initiator at 100℃ are determined by GPC. The results show that Iis a safe and efficient carbon-carbon bond initiator.