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  • Articles  (19)
  • Chemistry  (19)
  • Wiley-Blackwell  (19)
  • Springer
  • 2010-2014
  • 1980-1984  (10)
  • 1975-1979  (8)
  • 1965-1969  (1)
  • 1905-1909
  • Chemistry and Pharmacology  (19)
  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 241-247 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Quantitative analysis at 10-10g level ; Steroids in urine ; Amino acid fluorobutyrates (19 in 35 min) ; Installation of glass capillaries ; Connection to FM-ECD ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Glass capillary columns are ideal for analysis of urinary steroid profiles (i.e. the total steroid neutral fraction without prior separation into sub-groups).In this paper performance of both SCOT and wide-bore WCOT columns has been compared, resulting in no significant quantitative difference on urine extracts run as trimethylsilyl ether derivatives. However, because of increased efficiency the WB-WCOT column exhibited more sensitivity in measurement of small amounts of 11-ox-aetiocholanolone. Sensitivity of other steroids was greatly enhanced by use of either SCOT or WB-WCOT, leading to an almost tenfold increase over conventional packed columns (e.g. androsterone and aetiocholanolone 〈 40 μg per 24 h urine sample). A simple splitless injection system (based on a design of Dr. W. Greenaway, Oxford University) is presented.Experiments were also carried out using a SCOT column in conjunction with an FM-electron capture detector. Whilst efficiency was impaired due to the design of the detector, use of He (carrier) and N2 (make up gas) showed that several steroid derivatives could be easily measured at well below the 10-10 g level with much more rapid retention times than with a 1½m packed column. Highly successful separation of 19 amino acids (as fluoro-acyl derivatives) was achieved in 35 minutes using a SCOT (30 m) SP2100 column.
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  • 2
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Plant/Operations Progress 3 (1984), S. 86-88 
    ISSN: 0278-4513
    Keywords: Chemistry ; Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
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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
    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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  • 5
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Temperature Dependence Investigations of 31P Chemical Shifts of Trialkoxyphosphazene N-phosphoryldialkylestersThe 31P NMR spectra of a series of trialkoxyphosphazene-N-phosphoryldialkylesters, (RO)3P=N—P(O)(OR′)2, where R = R′ = Et; R = Et, R′ = Bu; R = Bu, R′ = Et; R = R′ = Bu; and R = R = R′ = Hex respectively, and of trichlorophosphazene-N-phosphoryldichloride were investigated at various temperatures. The temperature dependence of chemical shift of phosphorus belonging to the phosphazene group is multiplicately larger than that of phosphorus belonging to the phosphoryl group. This fact also could be confirmed for other simple phosphazene and phosphoryl compounds. As discussed this different temperature dependence of 31P chemical shift is not a consequence of the medium but of the molecular structure.
    Notes: Für eine Reihe von Trialkoxyphosphazen-N-phosphoryldialkylestern, (PO)3P=N—P(O)(OR′)2, wobei R = R′ = Et; R = Et, R′ = Bu; R = Bu, R′ = Et; R = R′ = Bu bzw. R = R′ = Hex waren, sowie für Trichlorphosphazen-N-phosphoryldichlorid wurden jeweils 31P-NMR-Spektren bei verschiedenen Temperaturen aufgenommen. Es zeigte sich, daß die Temperaturabhängigkeit der chemischen Verschiebung für den Phosphor der Phosphazen-Gruppierung um ein mehrfaches größer ist als die für den Phosphor der Phosphoryl-Gruppierung. Dies konnte auch allgemein für andere einfache Phosphazen- und Phosphoryl-Verbindungen bestätigt werden. Es wird diskutiert. daß diese unterschiedliche Temperaturabhängigkeit der 31P-chemischen Verschiebung nicht auf Medieneinflüsse, sondern auf die molekulare Struktur zurückzuführen ist.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 489 (1982), S. 131-138 
    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 Exocyclic 15N Labelled AmidochlorocyclotriphosphazenesSome exocyclic 15N labelled monoamidopentachlorocyclotriphosphazenes, N3P3Cl5X, and diamidotetrachlorocyclotriphosphazenes, N3P3Cl4X2, where X = 15NH2, 15NHMe, 15NMe2, or 15NHPh, were prepared, and the 31P- and 15N-NMR spectra were recorded. The chemical shift values δP and δN and the coupling constants 1JPN and 3JPN are discussed.
    Notes: Einige exocyclisch 15N-markierte Monoamidopentachlorocyclotriphosphazene, N3P3Cl5X, und Diamidotetrachlorocyclotriphosphazene, N3P3Cl4X2, wobei X = 15NH2, 15NHMe, 15NMe2 oder 15NHPh ist, wurden dargestellt und die 31P- und 15N-NMR-Spektren aufgenommen. Die chemischen Verschiebungen δP und δN und die Kopplungskonstanten 1JPN und 3JPN werden diskutiert.
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  • 7
    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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  • 8
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 31P and 195Pt N.M.R. Investigations on Diplatinum (I) Complexes of the Type [Pt2(μ-SPR2)2L2] (L = PR3, PhP(OPh)2, P(OPh)3, CNR)31P-, 195Pt-chemical shifts and 195Pt-31P- resp. 31P-31P-coupling constants of a series of doubly bridged diplatinum(I) complexes are reported. 31P-coordination chemical shifts of the terminal ligands of complexes of type [Pt2(μ-SPR2)2(P′R3′)2] and some of the various coupling constants are strongly influenced by the π-acceptor strength of these ligands. J(195Pt-195Pt) is found to change the sign among the series of complexes investigated. Thermal singlett triplet exitation giving rise to the paramagnetism of these complexes observed by preliminary EPR-measurements and confirmed by EHT-calculations is deduced from the large values of 2J(P-P′) and 3J(P′P′) as well as the unusually high temperature dependence of some coupling constants and other NMR features. The chemical stability of the doubly bridged core, the coordination shifts of the bridging phosphorus atoms and EHT-calculations suggest a view of aromaticity of the [Pt2(μ-SPR2)2](M-M) unit of these complexes.
    Notes: Es werden 31P-, 195Pt-chemische Verschiebungen und 195Pt31P-Kopplungskonstanten einer Reihe von doppelt verbrückten Diplatin(I)-Komplexen mitgeteilt. 31P-koordinationschemische Verschiebungen der ternären Liganden von Komplexen des Typs [Pt2(μ-SPR2)2(P′R3′)2] und verschiedene Kopplungskonstanten werden stark von der π-Akzeptor-Stärke dieser Liganden beeinflußt. J(195P-195Pt) wird innerhalb der Reihe der untersuchten Komplexe mit wechselndem Vorzeichen gefunden. Aus den großen Werten von 2J(Pt-P′) und 3J(P′P′) sowie der ungewöhnlich starken Temperaturabhängigkeit einiger Kopplungskonstanten und anderen NMR-Eigenschaften wird auf Paramagnetismus dieser Komplexe aufgrund thermischer Singlett-Triplett-Anregung geschlossen, der in vorläufigen EPR-Messungen gefunden und durch EHT-Rechnungen gestützt wird. Die chemische Stabilität des doppelt verbrückten Kerns, die koordinationschemischen Verschiebungen der Brückenphosphoratome und EHT-Rechnungen weisen auf Aromatizität der [Pt2(μ-SPR2)2](M-M)-Einheit dieser Komplexe hin.
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  • 9
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: N.M.R. Spectroscopic Investigations of N-Methyl-N-diethoxyphosphorylamido-chloro-cyclotriphosphazatrienesThe high resolution 31P-n.m.r. spectroscopy provides essential informations about the molecular structure of N-methyl-N-diethoxyphosphorylamido derivatives of the hexachlorocyclotriphosphazatriene. Whereas the compound N3P3Cl4[NCH3P(O)(OC2H5)2]2 possesses nongeminal structure, are the substituents in the compound N3P3Cl3[NCH3P(O)(OC2H5)2]3 geminally arranged. The calculated 31P spectra agrees closely with the observed.The interpretation of the 1H-n.m.r. spectra corresponds with that of the 31P-n.m.r. spectra.
    Notes: Die hochauflösende 31P-NMR-Spektroskopie liefert wesentliche Informationen über die Molekülstruktur von N-Methyl-N-diäthoxyphosphorylamido-Derivaten des Hexachlorocyclotriphosphazatriens. Während die Verbindung N3P3Cl4[NCH3P(O)(OC2H5)2]2 nichtgeminale Struktur besitzt, erweist sich die Verbindung N3P3Cl3[NCH3P(O)(OC2H5)2]3 als geminales Substitutionsprodukt. Die berechneten 31P-Spektren stimmen gut mit den experimentellen überein.Die Aussagen aus den 1H-NMR-Spektren stehen mit denen aus den 31P-NMR-Spektren in Einklang.
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  • 10
    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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