In the past years, many diazenyl compounds (i.e diazenecarboxamides, diazeniumdiolate prodrugs, diazenyl complexes etc.) have been prepared for the evaluation of their cytotoxic potential towards various cancer cell lines. Majority of them have shown promising cytotoxic activities even against several drug resistant cell lines. These derivatives have shown their effect by acting as alkylating agents, releasers of cytotoxic NO, targeting receptors like tyrosine kinase, EGFR or targeting enzymes like GST, AGT, CDKs etc. Their interaction with different receptors or enzymes leads to DNA damage, necrosis or apoptosis resulting in cell death. The present review will cover updated information on the synthetic methodologies and cytotoxic potential of diazenyl derivatives developed during the past years along with the recent developments. This may prove to be helpful for the researchers to develop novel anticancer drugs in future by molecular modifications of potential derivatives with better cytotoxic activities.