HNO (nitroxyl) is a biologically relevant unstable small molecule which rapidly dimerizes in aqueous solution. Thus, there is a need for HNO donors that can quickly release HNO “on demand”. Our group has developed a first generation family of HNO donors which generate HNO rapidly through photolysis. However, some competition from a photoredox side reaction reduces the utility of these molecules. The goal of this project was to explore the impact of incorporating a methyl substituent on the rate and selectivity of HNO generation. The poster will describe the studies completed to date on the synthesis and photochemistry of HNO donor.