1, 2-Bis(4-nitro-phthalimidomethyl)-1, 2-dicarba-closo-dodecaborane (12) (4-NP CBR) was synthesized by substitution reaction and alkyne insertion methodology using 4-nitrophthalimide, 1, 4-dichloro-2-butyne and decaborane as raw materials. The influences of solvent, molar ratio of raw materials and reaction temperature on the yield of 4-NP CBR were studied. The results indicated that under the optimized reaction conditions of molar ratio of 1, 4-bis(4-nitro-phthalimidomethyl)-2-butyne (4-NP BY) to bis-acetonitrile decaboraneof 1.2:1, toluene as solvent, heating at 100℃ for 16 h, the yield of 1, 2-bis(4-nitro-phthalimidomethyl)-1, 2-dicarba-closo-dodecaborane (12) was up to 51.2%. The product was characterized by means of FTIR, 1HNMR, 13CNMR and HR-MS techniques. Moreover, the UV absorption property of product was investigated. © 2018, Editorial Office of FINE CHEMICALS. All right reserved.