The commercial value of phenols is often reduced due to the presence of colored impurities. Several conventional techniques have been used for the purification of phenols. However, conventional purification techniques are tedious and make use of hazardous and expensive organic solvents. In this study, we present a new method for purification of an aged-discolored (orange) commercial 2,3-dimethyl phenol (2,3-DMP) reagent (97%) using supercritical fluid CO2 (SCF CO2), as an extraction solvent. A supercritical fluid extraction (SFE)/purification apparatus was constructed and purification of the reagent under different extraction conditions was investigated. Based on the differential solubility of the 2,3-DMP and the impurities in SCF CO2, the commercial reagent was successfully purified by SFE; the purified 2,3-DMP was a white solid of high purity (99.5%). The SFE method was also applied to purify a recently purchased batch of 2,3-DMP reagent. We found that the reagent purified by SFE was of a higher quality than a commercially available analytical standard.