To research the synthesis and performances of energetic compounds of bisisoxazole, three kinds of energetic compounds with low melting point, 5,5′-bis(azidomethyl)-3,3′-biisoxazole(2), [3,3′-biisoxazole]-5,5′-diylbis-(methylene)dinitrate(4) and [3,3′-biisoxazole]-4,4′,5,5′-tetrayl-tetrakis(methylene) tetranitrate(6) were synthesized via [3+2] cyclization reaction, nitration and azidation, using dichloroglyoxime, alkynol and propargyl bromide as starting materials, with a yield of 66%, 67% and 64%, respectively, and the structures of target compounds and intermediates were characterized by the means of IR, NMR and elemental analysis. The reaction mechanism of constructing bisisoxazole through two reactions of —C⁺ N—O^- and CC with 1,3-dipolar cycloaddition was discussed. The thermal behavior of compounds （2）, （4） and （6） were studied by DSC and TG. The melting temperature of compounds （2）, （4） and （6） are 77.46, 95.18 ℃ and 124.36 ℃. The starting temperature of thermal decomposition are 179.21, 165.34 ℃ and 168.69 ℃, respectively.