Synthesis and IR-spectral properties of alkyl isothiocyaoatocarboxylates are described. The isothiocyanates have been prepared by the thiophosgene method in aqueous as well as anhydrous solvents. The doublet of the v (C= O) band is interpreted to be due to the presence of two conformers. The population of the conformers is determined from the ratio of the apparent molar a bsorptivities, sa, of the computer-separated bands.