Aufgrund orientierender 31P‐NMR‐Untersuchungen der Reaktion von PSCl3 mit Hexamethyldisilazan (HMDS) wurden Darstellungsmethoden für das Trimethylsilylamid der Dichlorothiophosphorsäure 1, Me3SiNHP(S)Cl2 und das Diazadiphosphetidin 2, [Me3SiNHP(S)NSiMe3]2 ausgearbeitet. Beide Verbindungen wurden durch ihre IR‐, Raman‐, 31P‐NMR‐ und Massenspektren charakterisiert und ihr thermisches Verhalten untersucht. Bildung und Konstitution von 2 werden diskutiert und seine 1H‐ und 29Si‐Spektren mitgeteilt.
233ChemInform Abstract On the basis of 31P NMR spectroscopic study a method for the preparation of the trimethylsilylamide (I) and for the diazaphosphetidine (III) from the title compounds are developed. The 1:1 molar reaction in ether at room temp. gives the amide (I), while PSCl3 reacts with an excess disilazane (II) at 75 rc C to the diazaphosphetidine (III). The products are characterized by IR, Raman, 31P NMR,and mass spectroscopy, and their thermal behavior is studied.
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