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New perthiophosphonic acid anhydrides and the direct indication of the dimer-monomer equilibrium. NMR and X-Ray Studies

✍ Scribed by Haiko Beckmann; Gisbert Großmann; Gisela Ohms; Joachim Sieler

Publisher: John Wiley and Sons
Year: 1994
Tongue: English
Weight: 780 KB
Volume: 5
Category: Article
ISSN: 1042-7163
DOI: 10.1002/hc.520050113

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✦ Synopsis

New perthiophosphonic acid anhydrides (R-PSJ, with R = 2,4,6-tri-isopropyIphenyI and 2,4-di-tert-butyl-6-methylphenyl haw been prepared. For the latter case, the isolation of the monomer (n = I ) , the 2,4-di-tertbutyl-6-methyIphe~zyI-dithioxophosphorane, and both dimers (n = 2), cis-and trans-2,4-bis(2,4-di-tertbutyl-6-methylphenyl)-2,4-dithioxo-l, 3,2,4-dithiadiphosphetane, of one perthiophosphonic acid anhydride has been perfonned for the first time. The crystal structure of , !,4-di-tert-butyl-6-methylphenyl-di- thioxophosphorane

and of cis-2,4-bis(2,4,6-tri-isopropylphenyl)-2,4-dithioxo-l,3,2,4-dithiadiphosphetane has been determined. The new cis and trans dith iad iphosphetanm and d ith ioxophosphoranes as well as the known cowipouvzds (2,4,6-trimethylphmyl-PSJ2

and 2,4,6-tri-tert-butylphenyl-PS2 are characterized by solution and high resolution solid-state 3'P and I3C NMR spectroscopy. The existence of a dimer-monomer equilibrium ,is directly proved by 2 0 exchange 3JP 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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