© 2018 Bulgarian Academy of Sciences, Union of Chemists in Bulgaria.In this study, new piperazine derivatives were synthesized by the reactions of S-substituted-3-nitro-1,3-butadienes with some piperazine derivatives: (1-(2-furoyl)-, 1-(4-fluorobenzyl)-, 1-(3-fluorophenyl)- and 1-(1-tetrahydro-2-furyl)piperazine) in CHCl3 at room temperature. The structures of the new compounds were characterized by micro analysis, FT-IR, MS spectrometry, 1H- and 13C-NMR. The crystal structure analysis was performed on the synthesized compound 5d by using the X-ray diffraction method. The compound 5d crystallizes in the monoclinic space group P21/c with a = 12.5503(2) Å, b = 11.2039(2) Å, c = 14.1007(4) Å, Z = 4. The structure was solved by direct methods (SIR92) and refined to the residual index R1 = 0.031.