Phosphorus, Sulfur and Silicon and the Related Elements p. 117 - 132 (2000)
Update date:2022-09-26
Topics: Characterization Purification and Isolation Selection of Starting Materials Storage
Van Zyl, Werner E.
Fackler, John P.
2,4-Diaryl and 2,4-diferrocenyl-1,3-dithiadiphosphetane disulfide dimers, (RP(S)S)2, where R = Ph (1a), 4-C6H4OMe (1b) or ferrocenyl (Fc) (1c) react with a variety of alcohols, silanols, or trialkylsilylalcohols to form dithiophosphonic acids in a one-flask procedure. The generated acids have a relatively strong acidity which, upon deprotonation, facilitates the facile high yield conversion to monoanionic salts of the type [S2PR(OR′)]. The present study reports the systematic preparation of these salts with variation in both R and especially R′ groups. Compounds were characterized by 31P{1H} NMR spectroscopy and elemental analysis. High quality single crystals of (1a) were obtained from the slow cooling of a viscous melt which allowed for the X-ray crystal structure to be determined. Qualitative solubility data have been obtained for several of the isolated salts to provide valuable information for synthesis design, especially with regard to metal complexation. The title salts are effective precursors to obtain a series of new transition-metal complexes both in aqueous and non-aqueous solvents.
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