Disulfides 1-30 have been synthesized and their in vitro leishmanicidal activity has been evaluated. Compounds 18 (IC50 = 2.70 ± 0.044 μM), 19 (IC50 = 2.85 ± 0.02 μM), 20 (IC50 = 2.92 ± 0.01 μM), 26 (IC50 = 3.69 ± 0.01 μM), 21 (IC50 = 4.45 ± 0.029 μM), and 29 (IC50 = 4.46 ± 0.025 μM) showed a remarkable leishmanicidal activity if compared with standard pentamidine (IC50 = 5.09 ± 0.04 μM). This study has discovered a series of possible molecules as antileishmanial agents. A structure-activity relationship study has also been carried out. The structures of all the synthesized compounds were identified by using spectroscopic techniques, including 1H-NMR and EI MS.