A simple, fast, sensitive and selective spectrophotometric method has been developed based on the oxidative coupling reaction process, which depends on the determination of clonazepam (CZP) drug using an oxidizing agent sodium periodate (NaIO4) in the presence of a reagent, phenylephrine hydrochloride (PH-HCL), that uses the pink color of CZP at a wavelength of 495 nm. Where several factors aff ecting the color intensity and absorbance were studied, including the eff ect of color stability time, eff ect of the volume of the reagent, the eff ect of the volume of the oxidizing agent, order of addition and temperature. The calibration curve found to obey Lambert beer at range concentration (2–20 mg/L), while the limit of detection (LoD) (8. 9*10-2), limit of quantitation (LoQ) (2.6*10-2) and molar absorbance is 1.4 × 102 liters mol-1cm-1. The method was applied to pharmaceutical preparations (Tablet) and was found to characterize the best precision and accuracy. The standard methods not need any control of temperature and also not aff ected by interferences and henceforth successfully utilized to determine CZP in pharmaceutical preparations