Department of Chemistry, Institute of Science, Nagpur-440 0 11, India Manuscript received 29 July 1998, revised 23 April 1999, accepted 29 June 1999 Optimum conditions have been established for carrying out voltammetry at glassy carbon electrode for the anticancer drug 2-amino-4-(2-hydroxy-5-chlorophenyl)-6-phenylpyrimidine. The quantitative determination in terms of peak current magnitude (lp) in microamperes (µA) is found to be the best in 0.125 molar aqueous sodium carbonate buffer when GCE was held at -0.05 V for a period of 60s and then scanned at the rate of 50 mV s-1. Voltammogram shows two peaks at -1.39 V and -1.54 V (Ev values). Differential pulse polarography has also been carried out and 4-electron stepwise reduction is observed for the system in alkaline medium.