The (R)-BINOL-menthyl dicarbonates, one of the most important compounds in catalytic asymmetric synthesis, was synthesized by a convenient method. The molar heat capacities Cp,m of the compound were measured over the temperature range from 80 to 378 K with a small sample automated adiabatic calorimeter. Thermodynamic functions [HT–H298.15] and [ST–S298.15] were derived in the above temperature range with a temperature interval of 5 K. The thermal stability of the substance was investigated by differential scanning calorimeter (DSC) and a thermogravimetric (TG) technique.