Abstract:1,2-bis(4-nitro-phthalimidomethyl)-1,2-dicarba-closo-dodecaborane (12) was synthesized by substitution reaction and “alkyne insertion” methodology, using 4-nitro-phthalimide, 1,4-dichloro-2-butyne and decaborane as the raw material. The influence of the reaction agent, the mole ratio of raw material and temperature on the reaction were studied, and the best process conditions were obtained. When the reaction agent was toluene, n (1,4-bis(4-nitro-phthalimidomethyl)-2-butyne) : n (decaborane) was 1.2:1, reaction temperature was 100 oC, the yield of 1,2-bis(4-nitro-phthalimidomethyl)-1,2-dicarba–closo-dodecaborane was 51.2% when the reaction continued for 16 h. The products were characterized by FTIR, 1H-NMR, and 13C-NMR analysis，and their UV-absorption properties were also studied.