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  • 1975-1979  (3)
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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 437 (1977), S. 269-274 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Formation and Constitution of a Heterocyclic Phosphorus BetaineThe zwitter ionic 2,2,6,6-tetrakis(diethylamido)-4,4-Dioxo-1,3,5,2λ5,4λ5,6λ5-azadioxatriphosphorin (3) is formed as a cristalline byproduct in the reaction of octaethyl imidodiphosphoryl tetramide derivatives, {[(Et2N)2P(O)]2N}Y (Y = H, Na, SiMe3), with phosphorus(V) chlorides (PCl5, POCl3, ClP(O)(OEt)2). It is obtained from the primary reaction products in a secondary reaction. Its constitution was revealed by 31P-n.m.r.-spectroscopy and by synthesis of the 15N-labeled compound. From O-Diethoxyphosphorylated octaethyl imidodiphosphoryl tetramide the compound 3 is obtained only in presence of water traces and agents providing HCl like e. g. ClSiMe3 or ClP(O)(OEt)2.
    Notes: Bei der Umsetzung von Octaäthylimidodiphosphoryltetramid-Derivaten, {[(Et2N)2P(O)]2N}Y (Y = H, Na, SiMe3), mit Phosphor(V)-chloriden (PCl5, POCl3, ClP(O)(OEt)2) entsteht aus den primären Reaktionsprodukten in einer Folgereaktion das zwitterionische 2,2,6,6-Tetrakis(diäthylamido)-4,4-Dioxo-1,3,5,2λ5,4λ5,6λ5-azadioxatriphosphorin (3) als kristallines Nebenprodukt. Die Konstitutionsermittlung erfolgte mittels 31P-NMR-Spektroskopie und durch Synthese der 15N-markierten Verbindung. Aus dem O-Diäthoxyphosphorylierten Octaäthylimidodiphosphoryltetramid bildet sich 3 nur in Gegenwart von Wasserspuren und HCl-liefernden Reagenzien, wie ClSiMe3 oder ClP(O)(OEt)2.
    Additional Material: 1 Ill.
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  • 2
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Investigations on the Phosphorylation of Imidodiphosphoryl DerivativesDerivatives of esters and octaalkylamides of imidodiphosphoric acid, {[X2P(O)]2N}Y (X = OR, NR2; Y = H, Na, SiMe3, MgBr), react with phosphorus(V) chlorides exclusively under formation of O-phosphorylated products. No derivatives of nitridotriphosphoric acid are formed. O-Diethoxyphosphorylated phosphazenes, X2P(O)—N=PX2-O—P(O)(OEt)2, are obtained by using diethoxyphosphoryl chloride, (EtO)2P(O)Cl. Octaalkylamides react with PCl5 to form tetrachlorophosphonium compounds containing the PCl4 group chelate-like surrounded by the octaalkyl imidodiphosphoryl tetramide anion. The product of the reaction of octaalkyl imidodiphosphoryl tetramide sodium and POCl3 seems to have an analogous constitutions.
    Notes: Derivate von Estern und Octaalkylamiden der Imidodiphosphorsäure, {[X2P(O)]2N}Y (X = OR, NR2; Y = H, Na, SiMe3, MgBr), reagieren mit Phosphor(V)-chloriden ausschließlich unter Bildung O-phosphorylierter Produkte. Es entstehen keine Derivate der Nitridotriphosphorsäure. Mit Diäthoxyphosphorylchlorid, (EtO)2P(O)Cl, bilden sich O-Diäthoxyphosphorylierte Phosphazene, X2P(O)—N=PX2-O—P(O)(OEt)2. Die Octaalkylamide reagieren mit PCl5 zu Tetrachlorophosphoniumverbindungen, in denen die PCl4-Gruppe vom Octaalkylimidodiphosphoryltetramid-Anion chelatartig umgeben ist (IV). Eine analoge Konstitution scheint das Reaktionsprodukt von Octaäthylimidodiphosphoryltetramid-Natrium mit POCl3 zu haben.
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  • 3
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Constitution of the Trimethylsilyl Derivatives of Imidodiphosphoryl CompoundsEsters and dialkylamides of the imidodiphosphoric acid react with hexamethyl-disilazane to form trimethylsilyl derivatives. 1H-, 29Si-, and 31P-NMR data show the trimethylsilyl group to be bond to oxygen with rapid reversible exchange between both phosphoryloxygen atoms.
    Notes: Ester und Dialkylamide der Imidodiphosphorsäure reagieren mit Hexamethyldisilazan zu den Trimethylsilylderivaten. Aus 1H-, 29Si- und 31P-NMR-Daten folgt, daß die Trimethylsilylgruppe über Sauerstoff gebunden ist und einem schnellen reversiblen Austausch zwischen den beiden Phosphorylsauerstoffatomen unterliegt.
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