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  • 1975-1979  (11)
  • 1970-1974  (2)
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  • 1
    ISSN: 0021-8383
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: α-Substituted Phosphonates. XXXI. The Reaction of N,N,N′,N′-Tetramethyl Chloroformamidinium Chloride with P(III) CompoundsN,N,N′,N′-Tetramethyl chloroformamidiniumchloride (4) does not react with triethyl phosphite (TEP) or isopropyl diphenylphosphinate to give the expected bisphosphoryl derivatives 7 and 11, respectively, but primarily the monophosphorylated amidinium salts 6 and 10 respectively. The phosphine oxide 10 is stable, while 6 undergoes an elimination of ethyl chloride to the betain 8. Even under more drastic conditions the reaction of 4 or 8 with TEP does not lead to the expected bis(dimethylamino)bisphosphonate 7, but to the monoaminated bisphosphonate 1, involving a reduction step. Similar reduction has been observed under mild conditions in Michaelis-Arbusov reaction of dichloromethylenimonium chloride, yielding the expected trisphosphonate 2 and the bisphosphonate 1 as a by-product.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 411 (1975), S. 148-152 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Properties of Lineary PhosphorylchlorphosphazenesThe phosphorylchlorphosphazenes, Cl2(O)P - [N=PCl2]n - Cl, (n = 1, 2, 3) react like POCl3 with hexamethyldisilazan forming silylamides, Cl2(O)P - [N = PCl2]n - NHSi(CH3)3, (n = 0, 1, 2, 3). From these are obtained the phosphorylchlorphosphazenes by reaction with PCl5 containing one group  - N = PCl2 more.
    Notes: Die Phosphorylchlorphosphazene, Cl2(O)P - [N=PCI2]n - Cl, (n = 1, 2, 3) reagieren ebenso wie POCl3 mit Hexamethyldisilazan zu den Silylamiden, Cl2(O)P - [N=PCl2]n - NHSi(CH3)3, (n = 0, 1, 2, 3), aus denen mit PCl5 die um eine Phosphazengruppe verlängerten Phosphorylchlorphosphazene erhalten werden.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the „HCl- Condensation“ of Phosphorus OxytriamideThe reaction of HCl with phosphorus oxytriamide suspended in ether leads to highly cross-linked imidopolyphosphates. By substitution of amido group by chlorine atoms amidochlorides of phosphoric acid are also formed which are soluble in ether. Only traces of oligomeric μ-imidophosphoric acid amides are obtained. The intermediate formation of phosphorylimide amide, OP(=NH)NH2, and phosphoryl imide chloride, OP(=NH)CI, is assumed to explain the experimental results.
    Notes: Die Reaktion von HCl mit Phosphoroxidtrimid in ätherischer Suspension führt zur Bildung stark vernetzter Imidopolyphosphate. Durch Substitution von Amidgruppen durch Chloratome entstehen außerdem ätherlösliche Amidchloride der Phosphorsäure. Oligomere μ-Imidophosphorsäureamide werden nur in Spuren erhalten. Zur Interpretation der experimentellen Befunde wird die intermediäre Bildung von Phosphorylimidamid, OP(=NH)NH2, und Phosphorylimidchlorid, OP(=NH)CI, angenommen.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 430 (1977), S. 227-233 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Imidodiphosphoric Acid EstersImidodiphosphoryl tetrachloride reacts with aliphatic alcohols (C1-C3) as well as with sodium phenolate to form tetraalkylesters or tetraphenylesters of the imidodiphosphoric acid, resp. The tetraalkylesters (alkyl = methyl, ethyl, n-propyl) are also formed by reaction of trichlorphosphazene phosphoryldichloride, Cl3P=N—POCl2, with the corresponding alcohols. The purification of the esters can be reached by destillation of their silyl derivatives followed by desilylation. The esters are associated by intermolecular O…H…O hydrogen bonds.
    Notes: Imidodiphosphoryltetrachlorid reagiert mit Alkanolen (C1-C3) zu den Tetraalkylestern und mit Natriumphenolat zum Tetraphenylester der Imidodiphosphorsäure. Die Tetraalkylester (Alkyl = Methyl, Äthyl, n-Propyl) werden auch bei der Umsetzung von Trichlorphosphazenphosphoryldichlorid, Cl3P=N—POCl2, mit den entsprechenden Alkoholen gebildet. Die Reinigung der Ester gelingt durch Destillation ihrer Silylderivate und deren anschließender Desilylierung. Die Ester sind über intermolekulare O … H … O-Wasserstoffbrücken assoziiert.
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  • 5
    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.
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  • 6
    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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  • 7
    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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  • 8
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Rearrangement of Alkyl Groups in N-phosphorylated AlkoxyphosphazenesWith diazomethane the tetrachloride as well as the tetraethylester of imidodiphosphoric acid form mixtures of O- and N-methyl derivatives. However diazoethane reacts with the tetraethyl ester only by O-ethylation yielding triethoxyphosphazene phosphoryl diethyl ester. Trichlorophosphazene phosphoryl dichloride reacts with methyl or ethyl alcohol in the molar ratio of 1:1 forming alkoxydichlorophosphazene phosphoryl dichlorides. The rearrangement of the O-alkyl derivatives to the N-alkyl isomers has been proved by 1H- and 31P-n.m.r. spectroscopy. In the case of triethoxyphosphazene phosphoryl diethyl ester it only occurs in the presence of ethyl iodide as catalyst.
    Notes: Sowohl das Tetrachlorid als auch der Tetraäthylester der Imidodiphosphorsäure bilden mit Diazomethan Gemische der O- und N-Methylderivate. Diazoäthan jedoch reagiert mit dem Tetraäthylester ausschließlich unter O-Äthylierung zum Triäthoxyphosphazenphosphoryldiäthylester. Trichlorphosphazenphosphoryldichlorid reagiert mit Methanol bzw. Äthanol im Molverhältnis 1:1 zu den Alkoxydichlorphosphazenphosphoryldichloriden. Die Umlagerung der O-Alkylderivate in die N-Alkylisomeren wurde mittels 1H- und 31P-NMR-Spektroskopie bewiesen. Im Falle des Triäthoxyphosphazenphosphoryldiäthylesters erfolgt sie nur in Gegenwart von Äthyljodid als Katalysator.
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 405 (1974), S. 109-112 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of Imidodiphosphoryl Tetrachloride with Phosphorus PentachlorideImidodiphosphoryl tetrachloride quantitatively reacts with PCl5 to form, HCl, POCl3, and Cl3P=N—POCl2. The mechanism of the reaction is discussed. Using 32P-labeled PCl5 was proved that the attack of the PCl5 to imidodiphosphoryl tetrachloride does occur about an oxygen atom.
    Notes: Imidodiphosphoryltetrachlorid reagiert mit PCl5 quantitativ zu HCl, POCl3 und Cl3P=N—POCl2. Der mögliche Reaktionsmechanismus wird diskutiert. Mit 32P-markiertem PCl5 gelang der Nachweis, daß der Angriff des PCl5 am Imidodiphosphoryltetrachlorid über ein Sauerstoffatom erfolgt.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 404 (1974), S. 219-224 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Properties of Imidodiphosphoric Acid AmidesTrichlorophosphazene phosphoryldichloride, Cl3P=N—P(O)Cl2, reacts with the stoichiometric amount of anhydrous formic acid resulting the tetrachloride of the imidodiphosphoric acid, Cl2(O)P—NH—P(O)Cl2. This tetrachloride yields with diazomethane the N-methyl compound, Cl2(O)P—N(CH3)—P(O)Cl2. The tetramide of the imidodiphosphoric acid and its octalkyl derivatives are obtained by reaction of the tetrachloride with ammonia, dimethylamine, and diethylamine, respectively.
    Notes: Trichlorphazenphosphoryldichlorid, Cl3P=N—P(O)Cl2, reagiert mit der stöchiometrischen Menge wasserfreier Ameisensäure zum Imidodiphosphorsäuretetrachlorid, Cl2(O)P—NH—P(O)Cl2. Mit Diazomethan bildet dieses das N-Methylderivat, Cl2(O)P—N(CH3)—P(O)Cl2. Durch Umsetzung mit Ammoniak, Dimethyl- bzw. Diäthylamin werden das Imidodiphosphorsäuretetramid sowie die entsprechenden Octaalkylderivate erhalten.
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