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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    ISSN: 0365-9496
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    ISSN: 0365-9496
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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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: N-Methyl-N-Diethoxyphosphorylamido Derivatives of Hexachlorocyclotriphosphazatriene. I. The Reaction of Hexachlorocyclotriphosphazatriene with Sodium N-Methylamidophosphoric Acid Diethyl Ester.The reaction of hexachlorocyclotriphosphazatriene with the sodium salt of 0, 0-diethyl-N-methylamido-phosphate in the molar ratios 1:1, 1:2, and 1:3 gives a mixture of partially substituted compounds. The N-methyl-N-diethoxyphosphorylamidoderivatives, N3P3Cl6-n[NCH3P(O)(OC2H5)]n (n = 1, 2, 3) were isolated in a pure form by preparative column chromatography. Compounds with a higher degree of substitution are not formed. The compounds are characterized by their molecular weights, elementary analysis, and TLC-Rf values.
    Notes: Die Reaktion von Hexachlorocyclotriphosphazatrien mit dem Natriumsalz des N-Methylamidophosphorsäurediäthylesters führt bei Raumtemperatur in den Molverhältnissen 1:1, 1:2 und 1:3 zu einem Gemisch partiell substituierter Verbindungen. Mit Hilfe der präparativen Säulenchromatographie konnten die N-Methyl-N-diäthoxyphosphorylamido-Derivate, N3P3Cl6-n[NCH3P(O)(OC2H5)2]n (n = 1, 2, 3); in reiner Form isoliert werden. Verbindungen höheren Substitutionsgrades wurden nicht erhalten. Die Verbindungen wurden durch ihre Molmassen, Elementaranalysen und die dünnschichtchromatographischen Rf-Werte charakterisiert und gesichert.
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  • 4
    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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  • 5
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: N-Methyl-N-Diethoxyphosphorylamido Derivatives of Hexachlorocyclotriphosphazatriene. II. Ammonoloyses of N-Methyl-N-Diethoxyphosphorylamido-ChlorocyclotriphosphazatrienesMonokis-[N-methyl-N-diethroxyphosphorylamido]-pentachloro-cyclotriphospha-zatriene and 2, 4-bis-[N-methyl-N-diethoxyphosphorylamido]-2, 4, 6, 6-tetrachloro-cyclotriphosphazatriene react with gaseous ammonia at room temperature to the corresponding diamino compounds, N3P3CL4-n[NCH3P(O)(OC2H5)2]n(NH2)2, (n = 1, 2). Total Exchange of the chlorine in the N-Methyl-Ndiethoxyphosphorylamido-derivatives, N3P3CL6-n[NCH3P(O)(OC2H5)2]n, (n = a, 2, 3), takes place during the reaction with liquid ammonia. Aminophosphazenes of the type N3P3[NCH3P(O)(OC2H5)2]n(NH2)6-n, (n = 1, 2, 3), are formed. The described aminocyclotriphosphazatrienes are characterized by their melting points, elementary analyses, molecular weights and the TLC-Rf-values.
    Notes: Monokis-[N-methyl-N-diäthoxyphorylamido]-pentachloro-cyclotriphosphazatrien und 2, 4-Bis-[N-methyl-N-diäthoxyphosphorylamido]-2,4,6,6-tetrachlorocyclotriphosphazatrien reagieren mit gasförmigem Ammoniak bei Raumtemperatur zu den entsprechenden diaminoverbindungen, N3P3CL4-n[NCH3P(O)(OC2H5)2]n(NH2)2, (n = 1, 2). Vollständiger Austausch des Chlors in den N-Methyl-N-diäthoxyphosphorylamido-Derivaten, S3P3CL6-n[NCH3P(O). (OC2H5)2]n, (n = 1, 2, 3). findet bei der Umsetzung mit flüssigem ammonial Statt. Es werden dabei Aminocyclophosphazene des Typs N3P[NCH33P(O)(OC2H5)2]n(NH2)6-n, (n = 1. 2. 3) gebildet, Die beschriebenen Aminocyclophosphazatriene werden durch ihre Schmelzpunkte, Elementaranalysen, Molmassen und die dünnschichtchromatographischen Rf-Werte charakterisiert.
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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: N-Methyl-N-Diethoxyphosphorylamido Derivatives of Hexachlorocyclotriphosphazatriens. IV N.M.R. Spectroscopic Investigations of the Products of the Ammonolysis of N-methyl-N-diethoxyphosphorylamindo-chloro-cyclotriphosphazatrienesBroad band 1H decoupled 31P n.m.r. spectra of products obtained by ammonolysis of N-methyl-N-diethoxyphosphorylamido-chloro-cyclotriphosphazatrienes provide essential hints at the constitution of these compounds. In this connection it may be easily demonstrated, both amino groups of N3P3Cl3[NCH3P(O)(OC2H5)2][NH2]2 as well as of N3P3Cl2[NCH3P(O)(OC2H5)2]2 [NH2]2 are arranged geminally. The spectral parameters were found and verified by simulation of spectra. The simulated 31P spectra agree closely with the observed ones. The conclusions from the 31P n.m.r. spectra are complemented by these from the 1H n.m.r. spectra.
    Notes: Protonenrauschentkoppelte 31P-NMR-Spektren der aus Ammonolysen von N-Methyl-N-diäthoxyphosphorylamido-chloro-cyclotriphosphazatrienen erhaltenen Verbindungen liefern wichtige Hinweise auf deren Konstitution. In diesem Zusammenhang läßt sich zeigen, daß die beiden Aminogruppen sowohl im N3P3Cl3[NCH3P(O)(OC2H5)2][NH2]2 als auch im N3P3Cl2[NCH3P(O)(OC2H5)2]2[NH2]2 geminal angeordnet sind. Die spektralen Parameter wurden auf dem Wege der Spektrensimulation gesichert.Die simulierten 31P-Spektren stimmen gut mit den experimentellen überein.Die Aussagen aus den 1H—NMR-Spektren ergänzen sich mit denen aus den 31P—NMR-Spektren.
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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: Phosphinophosphite - a Hydrolysis Product of ‘Phosphorous Suboxide, P4O’The hydrolytic degradation of polymer phosphorus suboxide, ‘P4O’ and of the P4-molecule in aqueous ethanolic sodium hydroxide leads in addition to wellknown substances to a compound containing two phosphorus atoms directly attached. By 31P-NMR spectroscopy it was identified as phosphinophosphite, [OP(O)(H)—PH2]-.
    Notes: Beim hydrolytischen Abbau des polymeren Phosphorsuboxids „P4O“ wie auch des P4-Moleküls in wäßrig-ethanolischer Natronlauge wird neben bereits bekannten Spezies eine zweikernige Phosphorverbindung gefunden, die mit Hilfe der 31P-NMR-Spektroskopie als Phosphinophosphit, [OP(O)(H)—PH2]-, identifiziert wurde.
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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: NMR Spectroscopic Studies of 15N Labelled Geminally Disubstituted CyclotriphosphazenesIt is demonstrated by means of some selected 15N labelled geminally disubstituted cyclotriphosphazenes, 15N3P3X4Y2 (X = Cl; Y = F, NH2, or SEt), as an example, that the coupling constants 1JPN may be of different signs. The absolute value of 1JPN is significantly influenced only by those substituents, which are bonded to the phosphorus nucleus directly concerned in the coupling. Also the 15N chemical shifts are only changed by substituents on directly bonded phosphorus atoms.
    Notes: Am Beispiel ausgewählter 15N-markierter geminal disubstituierter Cyclotriphosphazene, 15N3P3X4Y2 (X = Cl; Y = F, NH2, SEt), wird gezeigt, daß die Kopplungskonstanten 1JPN unterschiedliche Vorzeichen haben können. Auf die Größe von 1JPN haben nur jeweils diejenigen Substituenten einen merklichen Einfluß, die an den direkt an der Kopplung beteiligten Phosphorkern gebunden sind. Die 15N-chemischen Verschiebungen werden ebenfalls nur durch die Substituenten an unmittelbar benachbarten Phosphoratomen beeinflußt.
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 490 (1982), S. 121-128 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: NMR Spectroscopic Studies of 15N Labelled OxocyclophosphazanesThe completely 15N labelled cyclophosphazanes (15NMeP(OMe)O)3, (15NEtP(OEt)O)3, and (15NMeP(OMe)O)4 were prepared by rearrangement of the corresponding alkoxyphosphazenes and their 31P- and 15N-NMR spectra were investigated. On the case of the trimer compounds spectra of the ABB′XX′Y spin type were obtained; all coupling constants are relevant, and like the 15N chemical shifts they are found only by means of spectra simulations. The relative signs of the coupling constants 1JPN, 2JPP, 2JNN, and 3JPN were also obtained.
    Notes: Die vollständig 15N-markierten Cyclophosphazane (15NMeP(OMe)O)3, (15NEtP(OEt)O)3 und (15NMeP(OMe)O)4 wurden aus den entsprechenden Alkoxyphosphazenen dargestellt und sowohl 31P- als auch 15N-NMR-spektroskopisch untersucht. Bei den trimeren Verbindungen wurden Spektren vom Spintyp ABB'XX'Y erhalten; alle Kopplungskonstanten sind relevant, sie können wie die 15N-chemischen Verschiebungen nur auf dem Wege der Spektrensimulation erhalten werden. Es ergeben sich auch die relativen Vorzeichen für die Kopplungskonstanten 1JPN, 2JPP, 2JNN und 3JPN.
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  • 10
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: NMR Spectroscopic Studies of 15N Labelled PhenylamidochlorocyclotetraphosphazenesSome endocyclically 15N labelled phenylamidochlorocyclotetraphosphazenes, 15N4P4Cl7NHPh, 6,8-15N4P4Cl6(NHPh)2 and 4,8-15N4P4Cl6(NHPh)2, as well as the corresponding exocyclically 15N labelled compounds N4P4Cl715NHPh, 6,8-N4P4Cl6(15NHPh)2 and 4,8-N4P4Cl6(15NHPh)2 were prepared, and the 31P and 15N NMR spectra were recorded. In the case of the endocyclically labelled compounds it is possible to determine the relative signs of the coupling constants 1JPN by means of spectra simulation. In order to interprete the relatively large coupling constants 3JPN to the exocyclic nitrogen a Karplus diagram was calculated and discussed.
    Notes: Einige endocyclisch 15N-markierte Phenylamidochlorocyclotetraphosphazene, 15N4P4Cl7NHPh, 6,8-15N4P4Cl6(NHPh)2 und 4,8-15N4P4Cl6(NHPh)2, sowie die entsprechenden exocyclisch 15N-markierten Verbindungen N4P4Cl715NHPh, 6,8-N4P4Cl6(15NHPh)2 und 4,8-N4P4Cl6(15NHPh)2 wurden dargestellt und die 31P- und 15N-NMR-Spektren aufgenommen. Für die endocyclisch markierten Verbindungen lassen sich die relativen Vorzeichen der Kopplungskonstanten 1JPN über Spektrensimulationen bestimmen. Zur Erklärung der verhältnismäßig großen Kopplungskonstanten 3JPN zum exocyclischen Stickstoff wurde ein Karplusdiagramm berechnet und diskutiert.
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