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New perthiophosphonic acid anhydrides and the direct indication of the dimer-monomer equilibrium. NMR and X-Ray Studies
Authors:Haiko Beckmann  Gisbert Großmann  Gisela Ohms  Joachim Sieler
Abstract:New perthiophosphonic acid anhydrides (R-PS2)n with R = 2,4,6-tri-iso-propylphenyl and 2,4-di-tert-butyl-6-methylphenyl have been prepared. For the latter case, the isolation of the monomer (n = 1), the 2,4-di-tertbutyl-6-methylphenyl-dithioxophosphorane, and both dimers (n = 2), cis- and trans-2,4-bis(2,4-di-tertbutyl-6-methylphenyl)-2, 4-dithioxo-1, 3, 2, 4-dithiadiphosphetane, has been determined. The new cis and trans dithiadiphosphetanes and dithioxophosphoranes as well as the known compounds (2,4,6-trimethylphenyl-PS2)2 and 2,4,6-tri-tert-butylphenyl-PS2 are characterized by solution and high resolution solid-state 31P and 13C NMR spectroscopy. The existence of a dimer-monomer equilibrium is directly proved by 2D exchange 31P NMR spectroscopy. It is shown that the reaction of the monomer with methanol is faster than the reaction of the dimer with methanol.
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