Reaction of carbon tetrachloride with aqueous hydrogen peroxide in the presence of anhydrous iron(III) chloride was studied. Optimal conditions for the preparation of phosgene were found on the basis of analysis of the kinetic data and mechanism of the process. The reaction rate and yield (the latter reaching 95% in the stationary mode) are determined mainly by the amount of the heterogeneous catalyst. According to the experimental data, the reaction follows a radical mechanism.