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  • Wiley-Blackwell  (53)
  • Molecular Diversity Preservation International  (14)
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  • 11
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 107 (1974), S. 448-453 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thiophosphinic Amide Complexes of RheniumThe monomeric substitution products R2PNH2SRe(CO)4Br R=C6H5(3a), CH3 (3b)) with monodentate P—S—Re-linkage are obtained from the reaction of the thiophosphinic amides (C6H5PNH2S(1 a) or (CH3)2PNH2S(1 b) with [BrRe(CO)4]2 (2 a) according to equation (1). 3a and b eliminate CO according to equation (2) when warmed in C6H5 under formation of the probably polymeric tricarbonylrhenium complexes R2PNH2SRe(CO)4Br (R=C6H5 (4a), CH3 (4b)). In 4a, b, 1a or b are linked didentate via nitrogen and sulphur to rhenium. 4a and b are also formed from 1a and b and BrRe(CO)5 (2b). The newly prepared complexes 3a, b and 4a, b are characterized on the basis of their i. r., Raman and 1H n. m. r. spectra.
    Notes: Bei der Einwirkung der Thiophosphinsäureamide (C6H5)PNH2S (1 a) oder (CH3)2PNH2S (1 b) auf [BrRe(CO) 4]2 (2 a) erhält man gemäß Gl. (I) die monomeren Substitutionsprodukte R2PNH 2SRe(CO)4Br (R=C6H5 (3 a), CH3 (3 b) mit einzähniger P—S—Re-Verknüpfung. 3 a und b spalten beim Erwärmen in C6H6 gemäß Gl. (2) CO ab unter Bildung der wahrscheinlich polymeren Tricarbonylrhenium-Komplexe R2PNH2SRe(CO)3Br (R=C6H5 (4a), CH3 (4b). In 4a, b sind 1a bzw. b zweizähnig über Stickstoff und Schwefel an das Rhenium gebunden. 4a und b bilden sich auch aus 1 a und b und BrRe(cO)5 (2b). Die neu dargestellten Komplexe 3a, b und 4a, b werden IR-, Raman- und 1H-NMR-spektroskopisch charakterisiert.
    Additional Material: 2 Tab.
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  • 12
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 109 (1976), S. 3781-3792 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Asteranes, XIII Synthesis of Tetraasterane by Photodimerisation of 3,6-Dihydrophthalic AnhydrideThe cage dimeric tetraasteranetetracarboxylic dianhydride 8 as well as the open trans dimers 6 and 7 have been isolated among monomeric products (2-4) on irradiation 3,6-dihydrophthalic anhydride (1) in ether, acetone, and dioxane. Unsubstituted tetraasterane (pentacyclo-[6.4.0.02,7. 0.4,11 0.5,10]dodecane, 14, is obtained by degradation of tetraasterane-1,4,5,8-tetracarboxylic acid (12) with lead tetraacetate and N-chlorosuccinimide via the tetrachlorotetraasterane 13. The structures of 6 and 12 have been confirmed by X-ray analysis. The influence of substituents on fragmentation patterns of tetraasterane derivatives in the mass spectrometer is indicated.
    Notes: Bei der Belichtung von 3,6-Dihydrophthalsäure-anhydrid (1) in Äther, Aceton und dioxan werden neben monomeren Produkten (2-4) das käfigdimere Tetraasterantetracarbonsäure dianhydrid 8 sowie die offenen trans-Dimeren 6 und 7 isoliert. Der Abbau von Tetraasteran-1,4,5,8-tetracarbonsäure (12) mit Bleitetraacetat und N-Chlorsuccinimid ergibt über das Tetrachlortetraasteran 13, das unsubstituierte Tetraasteran (Pentacyclo[6.4.0.02,7 0.4, 110.5,10]dodecan,14, Die Strukturen von 6 und 12 wurden durch Röntgenanalyse bestätigt. Der Substituenteneinfluß auf den Zerfall von Tetraasteranderivaten im Massenspektrometer wird angedeutet.
    Additional Material: 2 Ill.
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  • 13
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 110 (1977), S. 3118-3125 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis of Bicyclo[3.3.1]nonane-2,4,7-trione by a New Method for β-Diketones from EstersBis(trimethylsilyl)acyloin enol ethers 7, available from esters by silylating acyloin condensation, react with phenyl(tribromomethyl)mercury to yield dibromocyclopropane derivatives 8. These are rearranged thermally into 2,3-Dibromo-1,3-bis(trimethylsilyloxy) olefins 9 from which 2-bromo-1,3-diketones 5 are obtained by hydrolysis. Dehalogenation is achieved with chromium(II) salts.
    Notes: Die aus Estern durch silylierende Acyloinkondensation zugänglichen Bis(trimethylsilyl)acyloin-enolether 7 reagieren mit Phenyl(tribrommethyl)quecksilber zu den Dibromcyclopropanderivaten 8. Diese lagern sich thermisch leicht in die 2,3-Dibrom-1,3-bis(trimethylsilyloxy)olefine 9 um, deren Hydrolyse zu 2-Brom-1,3-diketonen 5 führt. Die Enthalogenierung gelingt mit Chrom(II)-Salzen.
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  • 14
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The synthesis, characterization and liquid-crystalline (LC) properties of polysiloxanes containing side chains with terminal 2-fluorenyl groups and various lengths of spacers is reported. The polymers which have no flexible tail segment exhibit two smectic mesophases (SA and SE), as confirmed by polarizing microscopy, differential scanning calorimetry (DSC) and X-ray investigations; a nematic mesophase was not found. The clearing temperatures of the polymers (in the range between 120 and 170°C) are generally 70-80°C higher than the melting temperatures of the non-liquid-crystalline precursors with a terminal vinyl group. With increasing spacer length the less ordered SA phase is favoured and has been found in a temperature range of up to 100 K width. For polymers with an SE phase no glass transition was detectable with DSC. The synthesized polymers are examples of the strong potential of the fluorene core to form LC phases without further structural stabilization.
    Additional Material: 3 Ill.
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  • 15
    Electronic Resource
    Electronic Resource
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 191 (1990), S. 3107-3113 
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The synthesis of the liquid-crystalline polysiloxanes, 4a, 4b, 5a, 5b with 2,7-disubstituted fluorene units and of the related liquid-crystalline model compounds 2 and 3 is reported. Polymers 4a, 4b, 5a, 5b were prepared from monomers 2 and 3, respectively, and poly(hydrogenmethyl-siloxane) (PHMS) in a polymer-analogous reaction. The liquid-crystalline properties of the polymers and the corresponding low-molecular-weight compounds 2 and 3 were characterized by differential scanning calorimetry (DSC) and polarizing microscopy. Both compounds 2 and 3 show a smectic A and a smectic E mesophase, and the resulting polysiloxanes also exhibit smectic A- and smectic E-like textures but no nematic phase. The clearing point of the polymers is on the average by 100°C higher than that found for the low-molecular-weight compounds.
    Additional Material: 2 Ill.
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  • 16
    Electronic Resource
    Electronic Resource
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 178 (1977), S. 2785-2797 
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Isopropyl acrylate-2,3-14C and isopropyl acrylate-2,3-3H were polymerized using anionic initiators. The isotactic polymers were fractionated by fractional precipitation and characterized. The polymer fractions were hydrolysed to polyacrylic acids by trifluoroacetic acid. Aqueous solutions of these radioactive labelled polyacrylic acids were injected intravenously to mice in amounts of 40 to 100mg/kg. Distribution in organs and the excretion were studied. About two thirds of the dose were excreted within the first two days with a half-life of about 0,5 days. Further excretion took place with a half-life of about six weeks. Distribution in the organism was not uniform; the highest concentrations were found in spleen, bones, and liver, i.e. organs being parts of the reticuloendothelial system. A relationship between organ concentration and molecular weight of the polyacrylic acid was only observed in the spleen. Nine weeks after injection about 10% of the dose were still retained in the organism, mainly in the skeleton.
    Additional Material: 8 Ill.
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  • 17
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 13 (1990), S. 759-763 
    ISSN: 0935-6304
    Keywords: Thermal degradation ; N-methylcarbamate pesticides ; PTV injection ; On-column injection ; Splitless injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An experiment has been designed to study the thermal degradation of thermolabile compounds caused by various injection techniques. The four carbamate pesticides aminocarb, bendiocarb, carbaryl, and dioxacarb decompose thermally into methylisocyanate and the corresponding phenol. The carbamets and the phenols arising from them were separated on a 25 m SE-54 fused silica column; all compounds exhibited sharp peak shape indicating that the degradation observed took place completely within the injector.When cold on-column injection was employed no thermal degradation was observed whereas with hot splitless injection at 220°C decomposition of the carbamates was almost complete.PTV injection was found to produce intermediate results. When packed with glass wool and operated with glass wool and operated with starting temperatures lower than the boiling point of the solvent, decomposition was found to be almost complete. Applying isothermal conditions at 140°C (30°C above the boiling point of toluene) aminocarb and bendiocarb underwent only slight decomposition while carbaryl and dioxacarb were about half degraded. Results from PTV injection with an empty insert resembled those obtained using cold on-column injection and in this mode the application of temperatures up to 200°C resulted in no visible degradation. This can be explained by the short residence time of the sample in the injector.
    Additional Material: 4 Ill.
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  • 18
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 13 (1990), S. 697-701 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Injection techniques ; Deterioration by biological matrix ; Thermolabile compounds ; Pesticide analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An experiment was designed to study the long-term stability of analyses of pesticide residues in a complex food matrix using three different injection techniques. A spinach sample was spiked with five sulfur-containing pesticides of varying volatility and thermolability: azinphos-ethyl, dimethoate, methiocarb, ethiofencarb, and tri-allate. Tri-allate was selected as internal standard because of its thermal stability and its good chromatographic properties. Flame photometric detection resulted in chromatograms not subject to interference by peaks of compounds of the matrix. Starting with a clean and freshly, silanized injector an additional deactivation was found to occur on the first injection of a food sample resulting in an increased peak area for all pesticides in relation to tri-allate. Highest long-term stability was found with PTV injection. Best results for thermolabile carbamates were obtained using on-column injection. However, they were prone to faster deterioration.
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  • 19
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für die chemische Industrie 84 (1972), S. 74-74 
    ISSN: 0044-8249
    Keywords: Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 20
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 3 (1990), S. 459-469 
    ISSN: 0894-3230
    Keywords: Organic Chemistry ; Physical Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: N-[2,3-Bis(dimethylamino)cyclopropenylio]- and N-(tetramethylamidinio)pyridinium salts (trifluoromethanesulphonates and tetrafluoroborates) form 1:1 and 1:2 charge-transfer complexes with the pentakis(methoxycarbonyl)cyclopentadienide anion. The x-ray crystal structures of 1-[2,3-bis(dimethylamino)cyclopropenylio] pyridinium pentakis(methoxycarbonyl)cyclopentadienide tetrafluoroborate hydrate and of 1-[2,3-bis(dimethylamino)cyclopropenylio] pyridinium bis[pentakis(methoxycarbonyl)cyclopentadienide] were determined. In constrast, the tetra-cyano-p-quinodimethane (TCNQ) radical anion reacts with the first-mentioned salts by C—C bond formation to give novel dicationic salts. Thereby, the radical anion attacks the pyridinium γ-position of the N-(tetramethylamidinio)-pyridinium dication, but the three-membered ring of the N-[2,3-bis(dimethylamino)cyclopropenylio] pyridinium system.
    Additional Material: 6 Ill.
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