The measurement system for the detection of soot production as high-temperature pyrolysis of hydrocarbon fuels behind the reflected shock wave was established. By using the laser extinction method, the soot yields of toluene/argon mixtures were measured at high temperatures. The mole fractions of toluene were 0.25% and 0.5% while the pressures were approximate 2 and 4 atm. The temperatures ranged from 1 630 to 2 273 K. The dependence of soot yield on the temperature, pressure and fuel concentration was obtained. With the changes of temperature, the soot yield is a Gauss distribution. The soot yield increases as the pressure or fuel concentration increases. The maximum of soot yield was as high as 55%. The peak temperature of soot yield was not changed dramatically with the pressure. However, it changed from 1 852 to 1 921 K as the concentration of toluene increase from 0.25% to 0.5%. Moreover, we compared the soot yield between toluene and methylcyclohexane at pressure of 4 atm with fuel concertation of 0.5%. During the pyrolysis of methylcyclohexane, the peak temperature of soot yield was 2 045 K, which is about 135 K higher than that of toluene. However, the maximum soot yield of methylcyclohexane is only 1/8 of toluene. This work provides experimental reference for the research of soot particle emission in the engines and the mechanism of soot formation.