The phase boundaries of the CO2 + toluene, CO2 + acetone, and CO2 + ethanol binary systems have been measured via a dynamic synthetic method based on a fiber optic reflectometer. We focus on a wide range of concentration of CO2 from 0.2 to 0.9 in mole fraction with temperatures up to 572 K. The results are correlated by the Peng-Robinson equation of state (PR-EOS) with two interaction parameters, which shows that the PREOS can predict the phase boundaries of CO2 + toluene and CO2 + acetone well but cannot predict the phase boundaries of the CO2 + ethanol binary system.