A physicochemical study of 5-methylfurfural and tetrahydrofurfuryl alcohol (density, speed of sound, refractive index, surface tension, static permittivity, and viscosity) has been carried out under atmospheric pressure at temperatures from (278.15 to 338.15) K, while the vapor pressure was determined over a temperature range from (303.15 to 453.15) K. Furthermore, the ppT behavior has also been assessed over a temperature range from (283.15 to 338.15) K and a pressure range from (0.1 to 60.0) MPa. Results indicate that although values of speed of sound, molar free volume, and viscosity of tetrahydrofurfuryl alcohol are higher than for the rest of the furfural family, the free volume/molar volume ratio is smaller for 5-methylfurfural, indicating a better packing. Furthermore, VOC Character of the studied compounds is smaller than some traditional solvents.