Tetrathiophosphates III‡ and IIIb were identified in the reaction mixture by 31P NMR spectroscopy. Under the conditions studied, conversion was 78–85% for phosphorus and 87– 91% for thiols (the latter produce not only P–S and P= S bonds but also undergo oxidation to give dialkyl disulfides in 50–56% yields). The structure of compounds II‡ and IIb was confirmed by X-ray diffraction study, the data of elemental analysis, NMR and IR ...
