In the literature, the application of sonic anemometry has been limited to low subsonic Mach number, near-incompressible flow conditions. To the best of the authors’ knowledge, this paper represents the first time a sonic anemometry approach has been used to characterize flow velocity beyond Mach 0.3. Using a high speed jet, flow velocity was measured using a modified sonic anemometry technique in flow conditions up to Mach 0.83. A numerical study was conducted to identify the effects of microphone placement on the accuracy of the measured velocity. Based on estimated error strictly due to uncertainty in time-of-acoustic flight, a random error of 4 m s−1 was identified for the configuration used in this experiment. Comparison with measurements from a Pitot probe indicated a velocity RMS error of 9 m s−1. The discrepancy in error is attributed to a systematic error which may be calibrated out in future work. Overall, the experimental results from this preliminary study support the use of acoustics for high subsonic flow characterization.