The enantiometric purity of a vitamin D3 metabolite was determined more exactly by means of DSC than by ~ H-NMR. The melting curve was analysed by the partial area method based on the Schr6der-van Laar equation. In order to find a suitable method for separation(R)-2,3-dihydroxy-3--methylbutyl p-toluenesulfonate from the racemate, the phase diagram of the enantiomers was evaluated from DSC results. The occurrence of a racemic compound was confirmed by an X-ray diffraction investigation of the racemate and the enantiomers. The conclusions are discussed in comparison with the results of previous investigations.Both the drug activities and the undesired side-effects of enantiomers can differ extremely. The enantiomeric purity of bioactive components is therefore highly important, as was demonstrated by the Contergan disaster, for example.The enantiomeric purity of (R)-2,3-dihydroxy-3-methylbutyl p-toluenesulfonate HO~ H HaC--~ SO2--0"~< OH for the synthesis of (24R)-24, 25-dihydroxy-vitamin D3, and also that of the (S) enantiomer, were determined by 1H-NMR spectroscopy [1]. An enantiomeric purity of 94% or higher was determined. This result was not satisfactory. Therefore, the problem arose of finding a method of determining the purity more exactly. DSC seemed to be an interesting method.
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