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  • 1
    Electronic Resource
    Electronic Resource
    Electroreduction of organic compounds. 31. Electroreduction of 2- and 3-Chlorodibenzofuran in Deuterated Methanol (1998)
    New York, NY : Wiley-Blackwell
    Journal für Praktische Chemie/Chemiker-Zeitung 340 (1998), S. 430-436 
    Details
    ISSN: 0941-1216
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The cathodic reduction of dibenzofuran (2), 2-chlorodibenzofuran (4), and 3-chlorodibenzofuran (1) in deuterated methanol is investigated. The Birch-type reduction product 1,4-dibenzofuran (3) is formed from 1 via 2, whereas 2-chloro-1,4-dihydrodibenzofuran (5) is obtained as by-product besides 3 from 4 as starting compound. Deuterium is only incorporated into the reduction products if CH3OD or CD3OD but not if CD3OH are used. This observation is strongly indicative of a polar mechanism involving protonation rather than a radical mechanism with hydrogen atom abstraction to be operative.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prac.19983400505
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  • 2
    Electronic Resource
    Electronic Resource
    Kristall- und Molekülstruktur des Oxalsäure-bis(di-tert-butylmethylesters) (1976)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 109 (1976), S. 761-768 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal and Molecular Structure of Bis(di-tert-butylmethyl) OxalateThe structure of the title compound (4) has been determined from X-ray data and refined to R = 0.048. 4 crystallizes in the space group C2/c with lattice parameters a = 23.599(4) Å, b = 12827(1) Å, C = 15.272(2) Å and β = 108.89(2)°. - The molecule exhibits the unusual Z-configuration. Bond lenghts and angles show no particularities with the exception of the central C—C-bond which appears significantly short (a = 1.531 Å).
    Notes: Die Struktur der Titelsubstanz (4) wurde röntgenorgraphisch bestimmt und bis zu einem R von 0.048 verfeinert. 4 kristallisiert in der Raumgruppe C2/c mit den Zellparametern a = 23.599(4) Å, b = 12.827 (1) Å, c = 15.272(2) Å und β = 108.89(2)°. - Das Molekül liegt in der ungewöhnlichen Z-Konfiguration vor. Bindungslängen und -winkel zeigen mit Ausnahme der zentralen C—C-Bindung, die mit A = 1.531 Å relativ kurz erscheint, normale Werte.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19761090237
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  • 3
    Electronic Resource
    Electronic Resource
    Verdrillte Oxalsäurederivate Die Kristall- und Molekülstruktur von N,N,N′,N′-Tetramethyloxamid und -monothiooxamid (1977)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 110 (1977), S. 1159-1166 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Twisted Oxalic Acid Derivatives The Crystal and Molecular Structure of N,N,N′,N′-Tetramethyloxamide and -monothiooxamideThe structures of the title compounds (2 and 3) have been determined from X-ray data, and refined to R = 0.065 (2) and 0.057 (3) respectively. 2 crystallizes in the space group C2/c, 3 in the space group P21/c. - In the crystal 2 exhibits a configuration in which the two halves of the molecule are twisted by 71.4°. This angle amounts to 87.4° in 3.
    Notes: Die Strukturen der Titelsubstanzen (2 und 3) wurden röntgenographisch bestimmt und bis zu R-Werten von 0.065 (2) bzw. 0.057 (3) verfeinert. 2 kristallisiert in der Raumgruppe C2/c, 3 in der Raumgruppe P21/c. - 2 liegt im Kristall in einer Konfiguration vor, bei der die beiden Molekülhälften um 71.4° gegeneinander verdrillt sind; bei 3 beträgt dieser Winkel 87.4°.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19771100339
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  • 4
    Electronic Resource
    Electronic Resource
    Alkinylverbindungen von Übergangsmetallen, XXIX. Alkinyl[1,2-bis(diphenylphosphino)äthan]-Komplexe des Platins(II) (1975)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 108 (1975), S. 1511-1517 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Alkynul Compounds of Transition Metals, XXIX. Alkynyl[ethylenebis(diphenylphosphine)] complexes of Platinum(II)cis-[PtCl2(dpe)] reacts with alkali acetylides in liquid ammonia or liquid methylamine to yield nonionic monomers of the type cis-[Pt(C≡C̊)2(dpe)] (dpe = (C6H5)2P[CH2]2P(C6H5)2; R = H, CH3, C6H5). The analogous reaction with the divalent anion of o-diethynylbenzene, however, gives the polymeric cis-[Pt(C≡C)2C6H4(dpe)]n, cis-[Pt(C≡C)2C6H4(dpe)]n. With an excess of acetylide polymeric complexes of the type [K2Pt(C≡C̊)4(dpe)]n are precipitated.
    Notes: Durch Umsetzung von cis-[PtCl2(dpe)] mit Alkaliacetyliden in flüssigem Ammoniak bzw.flüssigem Methylamin werden nichtionische, einkernige Verbindungen des Typs cis-[Pt(C≡C̊)2(dpe)] (dpe = (C6H5)2P[CH2]2P(C6H5)2; R = H, CH3, C6H5) dargestellt. Eine analoge Reaktion mit dem zweiwertigen Anion des o-Diäthinylbenzols hingegen führt zu einem koordinationspolymeren cis-[Pt(C≡C)2C6H4(dpe)]n. Die Anwendung eines Acetylidüberschusses führt zu polymeren Komplexen des Typs [K2Pt(C≡C̊)4(dpe)]n.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19751080519
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  • 5
    Electronic Resource
    Electronic Resource
    Kristall- und Molekülstruktur von 5-tert-Butyldithioisophthalsäure-O,O′-diethylester (1977)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 110 (1977), S. 3792-3798 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal and Molecular Structure of O,O′-Diethyl 5-tert-ButyldithioisophthalateThe structure of the title compound (4) has been determined from X-ray data by means of direct methods and refined to R=0.057. 4 crystallizes in the space group P1¯.  -  The molecule is approximately planar; the interplanar angles between the plane of the benzene ring and those of the RO—CS-groups being 5.3° and 7.6°, respectively. The C=S bond length of 1.631 ± 0.002 Å points to a moderate double bond character.
    Notes: Die Struktur der Titelsubstanz (4) wurde röntgenographisch mit Hilfe der Direktmethode bestimmt und bis zu einem R von 0.057 verfeinert. 4 kristallisiert in der Raumgruppe P1¯.  -  Das Molekül ist fast eben gebaut; die Interplanarwinkel zwischen der Ebene des Benzolrings und denen der RO—CS-Gruppen betragen 5.3° und 7.6°. Die C=S-Bindungslänge von 1.631 ± 0.002 Å läßt auf einen mäßig ausgeprägten Doppelbindungscharakter schließen.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19771101209
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  • 6
    Electronic Resource
    Electronic Resource
    Bildung, Reaktionen, Kristall- und Molekülstruktur des cyclischen Sulfenylcarboxylates: 3-Oxo-3H-2,1-benzoxathiol-7-carbonsäure-methylester (1978)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 111 (1978), S. 1685-1692 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Formation, Reactions, Crystal and Molecular Structure of the Cyclic Sulfenylcarboxylate: Methyl 3-Oxo-3H-2.1-benzoxathiole-7-carboxylateOn heating of 2-(benzylsulfinyl)isophthalic acid (4) with acetic acid/acetic anhydride the cyclic sulfenylcarboxylates 7a and 7b are formed in an unexpected elimination reaction and rearrangement, respectively. 7a can be methylated to the title compound 7c. The structure of 7c has been determined from X-ray data and refined to R = 0.06. 7c crystallizes in the monoclinic system, space group P21/c. The molecule is nearly planar and reveals an intramolecular interaction which is reflected in a short S…‥O distance of 252 pm and an unusual IR spectrum (νCO 1750. 1650 cm-1).
    Notes: In einer unerwarteten Eliminierungsreaktion bzw. Umlagerung bilden sich beim Erhitzen von 2-(Benzylsulfinyl)isophthalsäure (4) mit Essigsäure/Essigsäureanhydrid die cyclischen Carbonsäure-Sulfensäureanhydride 7a und 7b. 7a kann zur Titelverbindung 7c methyliert werden. Die Struktur von 7c wurde röntgenographisch bestimmt und bis zu R = 0.06 verfeinert. 7c kristallisiert monoklin in der Raumgruppe P21/c. Das Molekül ist fast planar und zeigt intramolekulare Wechselwirkung, die an einem geringen S…‥O-Abstand (252 pm) und einem ungewöhnlichen IR-Spektrum (νCO 1750, 1650 cm-1) erkannt werden kann.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19781110505
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  • 7
    Electronic Resource
    Electronic Resource
    Thioketyle, 5. Isotrope ESR-Parameter von Thio- und Selenoketylen (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 2255-2277 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thioketyls, 5. Isotropic ESR Parameters in Thio- and SelenoketylsThe preparation of aliphatic and aromatic thio- and selenoketones and of some of their D-, 13C-, and 77Se derivatives is described. Most of these compounds yield persistent radical anions on one-electron electroreduction, which are studied by ESR spectroscopy.  -  The 13C coupling constants allow the conclusion that in thio- and selenoketyls the spin density is mainly located at the central carbon atom.  -  The observed temperature dependence of the coupling constants is in agreement with a planar geometry of the thioketyl molecule.
    Notes: Die Darstellung aliphatischer und aromatischer Thio- und Selenoketone sowie einiger ihrer D-, 13C- und 77Se-angereicherten Derivate wird beschrieben.  -  Bei der elektrochemischen Einelektronen-Reduktion liefern die meisten Vertreter persistente Radikalanionen, die ESR-spektroskopisch untersucht werden. Die gemessenen isotropen 13C-Kopplungskonstanten erlauben den Schluß, daß in der Thio- bzw. Selenoketyl-Gruppe die Spinpopulation am zentralen C-Atom am größten ist.  -  Die beobachtete Temperaturabhängigkeit der Kopplungskonstanten ist mit einer planaren Geometrie des Thioketyl-Moleküls in Einklang.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19801130620
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  • 8
    Electronic Resource
    Electronic Resource
    Thioketyle, 8. Radikalanionen von α-Thioxoketonen („Monothiosemidione“) (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2221-2228 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thioketyls, 8. Radical Anions of α-Thioxoketones (“Monothiosemidiones”)Radical anions (“monothiosemidiones”) 5 are obtained by in-situ electroreduction of α-thioxoketones. Conclusions about the spin density distribution are drawn from their ESR spectra. The unpaired electron is mainly located in the central CO—CS group. - Only 5a-g exhibit proton hfs splittings, and that for the protons of the thiobenzoyl but not of the benzoyl group. 13C-satellites of the CS- and CH3-carbon atoms are observed in the spectra of 5h-j. From the latter π-spin populations of the thiocarbonyl carbon atom of 0.82 (5h) and 0.54 (5j), respectively, are calculated.
    Notes: Durch in-situ-Elektroreduktion werden α-Thioxoketone in die Radikalanionen („Monothiosemidione“) 5 übergeführt. Aus deren ESR-Spektren lassen sich Rückschlüsse über die Aufenthaltswahrscheinlichkeit des ungepaarten Elektrons ziehen. Die zentrale CO—CS-Gruppe enthält den überwiegenden Teil der Spindichte. - Nur bei 5a-g treten meßbare Protonen-HFS-Aufspaltungen auf, und zwar für die Protonen der Thiobenzoyl- nicht aber der Benzoylgruppen. Bei 5h-j beobachtet man 13C-Satelliten der CS- und CH3-Kohlenstoffatome. Aus letzteren erhält man π-Spinpopulationen am Thiocarbonyl-C-Atom von 0.82 (5h) bzw. 0.54 (5j).
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821150618
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  • 9
    Electronic Resource
    Electronic Resource
    α-Oxo- und α-Thioxothioamide aus Methylketonen (1983)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 1983 (1983), S. 1116-1132 
    Details
    ISSN: 0170-2041
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: α-Oxo- and α-Thioxothioamides from Methyl KetonesMixtures of α-(chloro)sulfenyl chlorides 5 and trisulfides 6 are obtained from the reaction of thionyl chloride with methyl ketones in the presence of pyridine. From these mixtures as well as from the pure trisulfides 6, with amines the α-oxothioamides 1-4 are formed with good yields. Thionation of the thioamides 1 and 2 yields the deeply coloured α-thioxothioamides 16 and 17, the structure of which has been especially characterized by X-ray structure analyses.
    Notes: Bei der Reaktion von Methylketonen mit Thionylchlorid in Gegenwart von Pyridin entstehen Gemische aus α-(Chlor)sulfenylchloriden 5 und Trisulfiden 6, die - ebenso wie die reinen Trisulfide 6 - mit Aminen hohe Ausbeuten an α-Oxothioamiden 1-4 liefern. - Schwefelung der Thioamide 1 und 2 ergibt die tieffarbigen α-Thioxothioamide 16 und 17, deren Struktur insbesondere durch Röntgenstrukturanalysen charakterisiert wird.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jlac.198319830705
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  • 10
    Electronic Resource
    Electronic Resource
    Darstellung neuer vicinaler Tricarbonylverbindungen und einiger ihrer Schwefelanaloga (1983)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 1983 (1983), S. 1694-1711 
    Details
    ISSN: 0170-2041
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of New Vicinal Tricarbonyl Compounds and Some of Their Sulfur AnaloguesMesoxalamides 5, benzoylglyoxylamides 19, and pivaloylglyoxylamides 26 are prepared from the corresponding malonamides 4, benzoylacetamides 17 and pivaloylacetamides 24, respectively, by suitable oxidation reactions. Some of the sulfur analogues of 5, 19, and 26, including the first stable 2-thiomesoxalic acid derivative 11b, are also obtained. The spectroscopic properties of the compounds are discussed.
    Notes: Durch geeignete Oxidationsreaktionen gelingt die Überführung der Malonamide 4 in Mesoxalamide 5, der Benzoylacetamide 17 in Benzoylglyoxylamide 19 und der Pivaloylacetamide 24 in Pivaloylglyoxylamide 26. Auch Schwefelanaloga von 5, 19 und 26, darunter das erste stabile 2-Thiomesoxalsäurederivat 11b sind zugänglich. Die spektroskopischen Eigenschaften der dargestellten Verbindungen werden diskutiert.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jlac.198319831006
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