NMR INVESTIGATIONS ON DIASTEREOMERIC MIXTURES OF BIS(DIALKOXYTHIOPHOSPHORYL) SULFANES AND -POLYSULFANES CONTAININGsec. BUTOXY GROUPS. ASSIGNMENT OF31P,13C AND1H NMR SIGNALS IN A MIXTURE OF SEVEN DIASTEREOMERS USING SHIFT-CORRELATED 2D NMR SPECTRA

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Abstract
Synthesizing compounds of the structure diastereomeric mixtures were obtained. If possible, the 31P chemical shifts and P[sbnd]P coupling constants of the individual diastereomers were determined from the 31P NMR spectra of these diastereomeric mixtures. In addition, the mixture of the seven diastereomers of bis(di-sec. butoxythiophosphoryl)disulfane was analyzed using shift-correlated 31P[sbnd]31P {1H}, 13C-31P {1H}, 13C-1H {31P} and 1H-1H {31P) 2D NMR spectra. In this way, the 31P, 13C and 1H chemical shifts and the corresponding coupling constants were assigned to the diastereomers. The appearance of regions of similar chemical shift into which the 1H, 13C and 31P signals of identical atoms or atom groups can be classified is characteristic of all the diastereomeric mixtures investigated. These regions can be explained mainly by the symmetry relations of a molecule moiety (sBuO)2P(S)S[sbnd].