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1996 (1)
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 Title    Chemistry of the l,3>5-Triaza-2-phosphorin-4,6-diones, Part XII*. Synthesis and Characterization of 2-PhenyI-2-(/?-tolylthio)-l,3?5- trimethyI-l,3,5-triaza-4,6-dione-2-phosphorinonium Salts  
 Abstract    A . P in ch u k , Io n N e d a , C h ristian M üller, H o lg e r T h ö n n e ss e n , P e te r G. Jones, R e in h a rd S chm utzler The reaction of l,5-bis(trimethylsilyl)-l,3.5-trimethylbiuret (1) with/M olylsulfenyl chloride (2) furnished l-(/?-tolylthio)-5-trimethylsilyl-l,3,5-trimethylbiuret (3). In the reaction of 3 with phenyldichlorophosphine, 2-phenyl-2-(/?-tolylthio)-l,3,5-trimethyl-l,3,5-triaza-4,6-dione-2-phosphorinonium chloride (4) was formed. The same product was obtained from the reac­ tion of 2-phenyl-l,3,5-trimethyl-l,3,5-triaza-2/.3-phosphorin-4,6-dione (6) with p-tolylsulfenyl chloride (2). Compound 4 was isolated and characterized in the form of the hexachloroanti-m onate (4a). The spirophosphorane 2-phenyl-l,3,5-trimethyl-l,3,5-triaza-7,10-dioxa-8,9-perchlorobenzo-2As-phosphaspiro-[4.5]decan-4,6-dione (7) was prepared by the reaction of 4 with tetrachloroorthobenzoquinone. The new products were characterized by 'H -and 13C NMR spectroscopy, elemental analysis, 31P NMR spectroscopy in the case of 4a. 6 and 7, and mass spectrometry (4a). Single-crystal X-ray structural analyses of compounds 4a and 7 were conducted. The phosphorus atom of 4a has the expected tetrahedral geometry, with a rather short P-S bond of 204.9(2) pm. In 7 the geometry at phosphorus is almost ideal trigonal bipyramidal. Weak hydrogen bonds are formed from a C (:0) group to deuterochloroform of solvation. 
  Reference    Z. Naturforsch. 51b, 1494—1500 (1996); received February 13 1996 
  Published    1996 
  Keywords    1, 3, 5-Trimethyl-Substituted 1, 3, 5-Triaza-4, 6-dione-2-phosphorinonium Derivatives, Intram olecular Rearrangem ent, NMR Spectra, X-Ray 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-1494.pdf 
 Identifier    ZNB-1996-51b-1494 
 Volume    51