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  • Chemistry  (21)
  • Surface physics, nanoscale physics, low-dimensional systems
  • Wiley-Blackwell  (21)
  • 2000-2004  (5)
  • 1975-1979  (12)
  • 1970-1974  (4)
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  • Wiley-Blackwell  (21)
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  • 1
    Electronic Resource
    Electronic Resource
    Adsorption of tryptophan metabolites from physiological fluids on XAD-2 and determination by single ion monitoringPresented in part at the 10th International Symposium on Advances in Chromatography, Munich, Germany 3-6 November 1975.Abbreviations: T = tryptamine; IAA = indole-3-acetic acid; 5-HT = 5-hydroxytryptamine; 5-HIAA = 5-hydroxyindole-3-acetic acid; 5-HTP = 5-hydroxytryptophan; TP = L-tryptophan; EA = ethyl acetate; ACN = acetonitrile; PFPA = pentafluoropropionic anhydride. (1976)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 3 (1976), S. 91-96 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Endogenous tryptamine, 5-hydroxytryptamine, indoleacetic acid, 5-hydroxyindoleacetic and tryptophan have been recovered from urine and cerebro-spinal fluid by adsorption on XAD-2 resin (0.3 g). After adsorption of the sample on the resin, desorption with methanol provides a single fraction that contains all of these metabolites. The mass spectra of their pentafluoropropionyl derivatives show prominent ions at m/e 276 and 438 which are characteristic of indoles and 5-hydroxyindoles, respectively, a feature that allows the concurrent determination of all the components of each group by functional group analysis. A method has been developed to carry out single ion monitoring with the peak matching system of an Hitachi RMU-6H mass spectrometer. Identifications are based on the respective Kovats Indices and single ion monitoring of two characteristic ions per compound: tryptophan (m/e 276 and 347); tryptamine (m/e 276 and 289); indoleacetic acid (m/e 276 and 335); 5-hydroxytryptamine (m/e 438 and 451); 5-hydroxyindoleacetic acid (m/e 438 and 497). The method described illustrates the feasibility of assaying biogenic indoleamines and acidic metabolites, as well as their precursor amino acid on a single fraction in contrast to other standard fractionation methods. This is possible even if the mass spectrometer is not equipped with an alternating voltage accelerator provided that it has a peak matcher, although the lack of an alternating voltage accelerator requires two separate injections of the same sample, for quantification and identification; one for the indole profile and another for the 5-hydroxyindole profile. Both profiles can be verified by individual monitoring of the other confirmatory ions. With this method the use of a multiple ion detector would allow a simultaneous determination of all of these metabolites in one gas chromatograph mass spectrometer run.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200030210
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  • 2
    Electronic Resource
    Electronic Resource
    Synthesis of Silaproline, a New Proline Surrogate (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 807-811 
    Details
    ISSN: 1434-193X
    Keywords: Proline analogues ; Asymmetric synthesis ; Schöllkopf's method ; Silicon ; Amino acids ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The asymmetric synthesis of a new proline surrogate, incorporating the dimethylsilyl group at position 4 of proline using Schöllkopf's bis-lactim ether method, is described.
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  • 3
    Electronic Resource
    Electronic Resource
    Mechanisms of Cyclopalladation Reactions in Acetic Acid: Not So Simple One-Pot Processes (2000)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 2000 (2000), S. 217-224 
    Details
    ISSN: 1434-1948
    Keywords: Reaction mechanisms ; Cyclopalladation ; Acetic acid ; Pd-C bond stability ; Polynuclear species ; Palladium ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The processes operating during the synthetic cyclopalladation reactions of imines in acetic acid have been studied from a kinetico-mechanistic point of view. These reactions include a fast initial coordination to the palladium through the N-donor atom of the imine, followed by the proper C-H bond activation to produce the acetato bridged dimeric species. At this point, the lability of the bridging acetato groups, the hydrolysis of the C-Pd bonds, and/or the hydrolysis of C=N exo bonds contribute to the generation of dark red polynuclear compounds. The processes occurring after the C-H activation have been followed kinetically, both from palladium acetate plus imine, and the synthetically pure isolated acetato dimers as starting materials. The kinetic and activation parameters have been found identical within experimental error whatever the starting material was (k323 = 1.5 × 10-4 s-1; ΔH# = 51 kJ mol-1; ΔS# = -163 JK-1 mol-1 ΔV# = +19 cm3 mol-1 for the 4-ClC6H4-CH=N-CH2-C6H5 imine derivative 1a). Acidolysis of C-Pd bonds has been found to occur in these polynuclear species. When alternative monomeric Cbenzylic-Pd bond-containing complexes are possible follow ups of the reactions produce them as final dead-end complexes (k323 = 2.2 × 10-5 s-1; ΔH# = 61 kJ mol-1; ΔS# = JK-1 mol-1 ΔV# ≈ 0 cm3 cm-1 for the [2,4,6-(CH3)3]C6H2-CH=N-CH2-[2-(CH3]C6[H4] imine derivative 3d). The same study has been carried out with primary amines in order to check the validity of the data if C=N bond hydrolysis is taking place in the imine derivatives with exo C=N bonds. For complexes with similar type of metallacycles, the results agree reasonably well with the proposed mechanism [k323 = 1.2·10-4 s-1, ΔH# = 46 kJ·mol-1, ΔS# = -180 J·K-1mol-1, ΔV# = -16 cm3·mol-1 for the polynuclear formation of the C6H5-CH2-NH2 derivative 4e; k323 = 3.0·10-4 s-1, ΔH# = 55 kJ·mol-1, ΔS
    Additional Material: 1 Ill.
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  • 4
    Electronic Resource
    Electronic Resource
    Synthesis of New Seven-Membered Ring Cyclic Dipeptides From Functionalized β-Amino Acids (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 251-255 
    Details
    ISSN: 1434-193X
    Keywords: Amino acids ; coupling ; N-Substituted amide ; Cyclizations ; Cyclic dipeptides ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---A short synthesis of new, functionalized seven-membered ring cyclic dipeptides is described. After the coupling of N-protected β-amino acids to N-substituted α-amino tert-butyl esters, the protective groups of the terminal functions were removed and the cyclization took place diastereoselectively in the presence of the coupling agent BOP. Amide substitution was found to be effective in promoting the cyclization of linear dipeptides.
    Additional Material: 1 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Reductive Cleavage of Potential Cholinomimetics Thiadiazolidinones: A New Family of Spiro Compounds (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 675-680 
    Details
    ISSN: 1434-193X
    Keywords: Thiadiazolidinones ; Spiro compounds ; Thiazoles ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The design, synthesis and evaluation of a series of 1,2,4-thiadiazolidinones with potential muscarinic receptor binding properties has been performed. During the synthesis of the target compounds, we observed an interesting reductive cleavage of the thiadiazolidinone system which leads to the formation of the novel piperidine spiro triazine heterocycle. The synthesis, structural elucidation (NMR spectroscopy and X-ray diffraction) and biological evaluation of the new compounds are described. With the structures unequivocally established, a mechanism for the formation of the spiro compound is proposed.Supporting information for this article is available on the WWW under //http://www.wiley-vch.de/contents/jc_2046/2000/099462_s.pdf or from the author.
    Additional Material: 3 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    Direct solution of the isothermal gibbs-duhem equation by an iterative method for binary systems (1977)
    Hoboken, NJ : Wiley-Blackwell
    AIChE Journal 23 (1977), S. 393-395 
    Details
    ISSN: 0001-1541
    Keywords: Chemistry ; Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/aic.690230329
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  • 7
    Electronic Resource
    Electronic Resource
    Darstellung, Temperaturverhalten und Kristallstruktur von BiF3 (1977)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 436 (1977), S. 105-112 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation, Temperature Behaviour, and Crystal Structure of BiF3Orthorhombic BiF3 was prepared from BiOCl and HF at 300°C through elimination of oxygen. Thermal analysis showed no transformation up to the melting point of 757°C. The orthorhombic structure of BiF3 can, however, transform into the structure of Tysonit in presence of a small amount of oxygen. The single-crystal X-ray structure determination (553 reflexions, R = 0.050) demonstrated that BiF3 is isostructural with the rare-earth trifluorides of the YF3 type (Pnma). The coordination polyhedron around Bi can be described in terms of a slightly distorted square-antiprisma (CN = 8).
    Notes: Orthorhombisches BiF3 wurde aus BiOCl und Fluorwasserstoff bei 300°C unter Ausschluß von Sauerstoff dargestellt. BiF3 zeigt bis zum Schmelzpunkt bei 757°C keine Phasen-umwandlung. Die orthorhombische BiF3-Struktur kann durch sehr geringe Sauerstoffgehalte in die Tysonitstruktur umgewandelt werden. Die Einkristall-Röntgenstrukturanalyse (553 Reflexe, R = 0,050) ergab, daß BiF3 isotyp mit den Selten-Erd-Trifluoriden vom YF3-Typ (Pnma) ist. Die Koordinationsverhältnisse um Bi können mit Hilfe eines leicht verzerrten quadratischen Antiprismas (KZ = 8) beschrieben werden.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19774360112
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  • 8
    Electronic Resource
    Electronic Resource
    The effect of the molecular weight on thermal degradation of fractionated PVC (1975)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 46 (1975), S. 81-87 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Ein technisches PVC und eine andere in Substanz bei 40°C hergestellte Probe wurden nach der Lösungsmethode mit Methanol-Cyclohexanon-Gemischen fraktioniert. Beide Polymere geben Fraktionen mit gleicher Taktizität, aber verschiedenen Molekulargewichten. Der thermische Abbau wurde bei 175, 180 und 185°C durch fortlaufende Bestimmung des abgespaltenen HCl in einem Leitfähigkeitsapparat untersucht. Je niedriger das Molekulargewicht ist, desto größer ist die Abbaugeschwindigkeit; dies gilt aber nur für Polymere mit Molekulargewichten bis etwa 60 000 oder 90 000; oberhalb dieser Werte ist die Abbaugeschwindigkeit vom Molekulargewicht unabhängig. Die Spektren der Proben mit dem gleichen Abbauumsatz zeigen, daß die Verteilung der Polyensequenzen gleich ist und daher nicht vom Molekulargewicht beeinflußt wird.
    Notes: A commercial PVC and another one prepared in bulk at 40°C were fractionated by means of fractional solution method using cyclohexanone-methanol mixtures. Both fractionations resulted in two sets of fractions. Their thermal degradation at 175, 180 and 185°C was followed by means of a conductivity cell which allows a continuous titration of the evolved HCl. The results showed that the lower the molecular weight the higher the degradation rate was; nevertheless, this relationship is only valid up to molecular weights of 60 000 to 90 000, from which the degradation rate appeared to be independent on the molecular weight. The UV-visible spectra of the degraded polymers suggest a similar polyene sequence distribution for all the fractions which accounts for a similar mechanism of degradation in contrast to what happens to fractions with different tacticity.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/apmc.1975.050460108
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  • 9
    Electronic Resource
    Electronic Resource
    The influence of the tacticity on thermal degradation of PVC. III. Verification by ozonization of degraded samples (1979)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 75 (1979), S. 215-222 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Mit abgebauten PVC-Proben verschiedener Taktizitäten wurden zwei Reihen Ozonolysereaktionen mit 1 und 24 h durchgeführt. Bei der Ozonolyse wurde die Verteilug der Polyensequenzlängen durch UV-Vis-Spektroskopie verfolgt. Die Kettenspaltungszahl der analysierten Proben wurde durch Bestimmung des Molekulargewichtes vor und nach der Ozonolyse berechnet.Die beobachtete Zunahme der kürzeren Polyensequenzen im Vergleich zu längeren Polyensequenzen bei der Ozonolyserektion hängt von den syndiotaktischen Sequenzen ab. Es wurde andererseits gefunden, daß bei PVC die Zahl der Kettenspaltungen nach der vollständigen Ozonolyse um so kleiner ist, je größer der Anteil von taktischen Sequenzen ist.
    Notes: Two sets of ozonization reactions, for 1 h and 24 h respectively, have been carried out at -20°C on degraded samples of PVC having different contents of tactic sequences. The evolution of the polyene sequences distribution with the ozonization was followed by UV-Visible spectroscopy. The number of chain scissions of ozonized samples was calculated from the number average molecular weight measurements before and after ozonization.The observed increase of short polyenes relative to the long polyenes with ozonization was found to depend markedly on the content of syndiotactic sequences. On the other hand, the number of chain scissions after total ozonization was found to be the higher the lower the content of tactic sequences in PVC samples is.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/apmc.1979.050750116
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  • 10
    Electronic Resource
    Electronic Resource
    The influence of the tacticity on thermal degradation of PVC. II. New results obtained with fractionated polymers (1975)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 45 (1975), S. 177-184 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Bei 40, 0 und -50°C hergestellte PVC-Proben wurden nach verschiedenen Methoden fraktioniert. Die Fraktionen wurden durch Viskositätsmessungen und IR-Spektroskopie charakterisiert. Der thermische Abbau der Fraktionen wurde bei 175, 180 und 185°C durch fortlaufende Messung des abgespaltenen Chlorwasserstoffs in einem Leitfähigkeitsapparat untersucht. Die kinetischen Ergebnisse und die Spektren der Proben zeigen, daß die syndiotaktischen Sequenzen die Ursache für den schnellen Abbau sind und daß dabei lange Polyensequenzen entstehen, wie schon früher bei unfraktionierten Polymeren ermittelt wurde.
    Notes: PVC samples prepared in bulk at 40, 0, and -50°C were fractionated by different methods. The samples were characterized by viscosimetric measurements and by IR spectroscopy in order to determine the tacticity. The thermal degradation of the samples was studied at 175, 180, and 185°C by means of continuous measuring of the evolved HCl in a conductivity apparatus. From the kinetic results and the UV-visible spectra recorded on equally degraded samples follows that syndiotactic sequences give rise to high degradation rates as well as to long polyene sequences in agreement with results previously obtained with unfractionated polymers.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/apmc.1975.050450113
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