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  • Chemistry  (10)
  • Analytical Chemistry and Spectroscopy  (5)
  • 1990-1994  (2)
  • 1985-1989  (2)
  • 1970-1974  (6)
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Years
Year
  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 103 (1970), S. 2885-2893 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the knowledge of the Organo Phosphorus Compounds, XII. The Reaction of Thiophosphoryl Derivatives with Grignard Reagents and the Analysis of the Mixtures by n. m. r. Double-Resonance MethodsThe reaction of t-C4H9MgCl with (CH3)nP(S)X3-n (n = 0, 1, 2; X = Cl, Br) and of CH3MgX′ (X′ = Br, J) with (t - C4H9)nP(S)X3 - n ( 1, 2; X = Cl, Br) is investigated. The complex mixtures obtained are favourably analysed double-resonance methods as f. i. in the case of the formation of CH3(t-C4H9)P(S)J.
    Notes: Die Einwirkung von tert.-Butylmagnesiumchlorid auf (CH3)nP(S)X3-n (n = 0, 1, 2; X = Cl, Br) und die Reaktion von CH3MgX′ (X′ = Br, J) mit (t-C4H9)nP(S)X3-n (n = 1, 2; X = Cl, Br) werden untersucht. Komplexe Reaktionsgemische lassen sich vorteilhaft mittels NMR-Doppelresonanztechniken analysieren, wie u. a. am Beispiel der Bildung von (CH3(t-C4H9)-P(S)J gezeigt wird.
    Additional Material: 4 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 103 (1970), S. 2114-2121 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Knowledge of Organophosphorus Compounds, X. Synthesis and Properties of tert-Butyl Substituted Thiophosphoryl HalidesSynthesis and properties of the tert-Butylthiophosphorylhalides (t—C4H9)nP(S)X3-n (X = Cl, Br; n = 1, 2), the asymmetric compounds R(t—C4H9)P(S)Br (R = CH3, C2H5, i—C3H7) and RP(S)Br2 (R = CH3, i—C3H7) are described, i. r. - and n. m. r. -data are reported.
    Notes: Darstellung und Eigenschaften von tert. -Butylthiophosphorylhalogeniden (t—C4H9)nP(S)X3-n (X = Cl, Br; n = 1,2), der asymmetrischen Verbindungen R(t—C4H9)P(S) Br (R = CH3, C2H5, i—C3H7) und RP(S)Br2 (R = CH3, i—C3H7) werden beschrieben, IR- und NMR-spektroskopische Daten angegeben.
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  • 3
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Nuclear Magnetic Resonance Investigations of Pentafluorphenyl-substituted Silanes, I. Correlations of Chemical Shifts, Coupling Constants, and (p-d)π-InteractionsThe 19F n.m.r. spectra of silanes (C6F5)n SiX4-n (X = F, Cl, Br, H, Alkyl, C6H5; n = 1-4) and disilanes C6F5(CH3)2 SiSi(CH3)2 X (X = CH3, C6F5) are analysed Using the ΦF* and JFF values π-acceptor properties of silicon are discussed as function of substituents.
    Notes: Es werden Silane des Typs (C6F5)n SiX4-n (X =; F, CI, Br, H, Alkyl, C6H5; n = 1 - 4) sowie die Disilane C6F5 (CH3)2SiSi (CH3)2 X (X = CH3, C6F5) 19F-NMR-spektroskopisch untersucht. Anhand der ΦF*- und JFF-Werte wird die π-Akzeptorwirkung des Siliciums in Abhängigkeit von der Art der Substituenten und vom Substitutionsgrad diskutiert.
    Additional Material: 4 Ill.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 103 (1970), S. 2274-2280 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Knowledge of Organophosphorus Compounds, XI. Preparation and Properties of Methyl-tert-butylthiophosphinic Acid DerivativesSynthesis and properties of the methyl-tert-butylthiophosphinic acid derivatives CH3(t-C4H9)P(S)X (X = Br, OR, OH, ONa, O-Chinin. H, OZn/2, SNa, Cl and t-C4H9) are described. I. r. and n. m. r. data are reported.
    Notes: Darstellung und Eigenschaften der Methyl-tert.-butyl-thiophosphinsäure-Derivate des Typs CH3(t-C4H9)P(S)X (X = Br, OR, OH, ONa, O-Chinin H. OZn/2, SNa, Cl und t-C4H9) werden beschrieben und ihre IR- und NMR-spektroskopischen Daten mitgeteilt.
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  • 5
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 6 (1974), S. 66-72 
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Long range 5J(FH) and 6J(FH) couplings were observed for silanes of the type (C6F5)nSiR4-n (n = 1, 2, 3; R = alkyl, aryl) and disilanes C6F5[Si(CH3)2]2R (R = CH3, C6F5). A characteristic increase in line width for 19F-NMR spectra of (C6F5)nSiR4-n(n ≧ 2) is thought to be due to spin systems of the type ([AC]2B)n or ([AX]2M)n with intra-annular couplings between ortho-fluorine atoms of neighbouring ring systems.
    Notes: Longrange-Kopplungen des Typs 5J(FH) und 6J(FH) werden bei Silanen des Typs (C6F5)nSiR4-n (n = 1, 2, 3; R = Alkyl, Aryl) sowie den Disilanen C6F5[Si(CH3)2]2R (R = CH3, C6F5) beobachtet. Eine typische Linienverbreiterung der Fluor-resonanzspektren von (C6F5)nSiR4-n (n ≧ 2) wird auf Spinsysteme des Typs ([AC]2B)n bzw. ([AX]2M)n mit interanularen Kopplungen der ortho-Fluor-atome benachbarter Ringe zurückgeführt.
    Additional Material: 15 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 6 (1974), S. 374-379 
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The isomeric compounds 1,2-difluoro-4,5-dimethylthiobenzene and 1,4-difluoro-2,3-dimethylthiobenzene were synthesised from CH3SNa and 1,2,4,5-tetrafluorobenzene and 1,2,3,4-tetrafluorobenzene, respectively. The structures of both the C6H2F2(SCH3)2 isomers were determined by NMR spectroscopic methods. The subspectral breakdown of an [AMX3]2 spin system is shown for the limiting case of vanishing long range coupling constants.
    Notes: Aus CH3SNa und 1,2,4,5- bzw. 1,2,3,4-Tetrafluorobenzol wurden 1,2-Difluor-4,5-dimethylthiobenzol bzw. 1,4-Difluor-2,3-dimethylthiobenzol dargestellt. Die Struktur der beiden C6H2F2(SCH3)2-Isomeren wurde durch kernresonanz-spektroskopische Methoden bestimmt. Der subspektrale breakdown des [AMX3]2-Spinsystems wird für den Sonderfall verschwindender long-range-Kopplungen abgeleitet.
    Additional Material: 6 Ill.
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  • 7
    ISSN: 0044-2313
    Keywords: Aminomethylphosphine oxides ; synthesis ; 31P{1H}-NMR controlled titrations ; stability constants ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Aminomethylphosphinoxide: Synthese, Dissoziations- und Stabilitätskonstanten, 31P-{1H}-NMR-kontrollierte TitrationenDie Titelverbindungen werden durch Gabriel-Synthese nach bekannten und verbesserten Verfahren erhalten. Durch neue Methoden der 31P{1H}-NMR-kontrollierten Titration werden Dissoziations- (gegeben als Basizitäts- und Aciditäts-) sowie Stabilitätskonstanten erhalten. Dynamisch gemittelte und ionenspezifische Chemische Verschiebungen δP werden abgeleitet.
    Notes: The title compounds are prepared via Gabriel-synthesis following known or improved procedures. Novel methods using 31P{1H}-NMR controlled titrations of aminomethylphosphine oxides lead to dissociation constants (given as basicity or acidity constants resp.) and to stability constants. Dynamically averaged and ion specific chemical shifts δP were derived.
    Additional Material: 8 Ill.
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  • 8
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 27 (1989), S. 470-475 
    ISSN: 0749-1581
    Keywords: Solid-state NMR ; Aminophosphonic acids ; Crystallography ; Shielding tensors ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: High-resolution 31P, 15N and 13C NMR spectra have been obtained for nine solid aminophosphonic acids under conditions of high-power decoupling, cross-polarization and magic-angle spinning. The NMR evidence shows that the asymmetric unit is a single molecule in all cases, which is consistent with the available diffraction studies. Phosphorus-31 shielding tensor components determined from static and slow-spinning MAS spectra are given for a number of the compounds.
    Additional Material: 5 Ill.
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  • 9
    ISSN: 0749-1581
    Keywords: Ethanol ; Deuterium ; SNIF-NMR ; 1H NMR ; 13C NMR ; 31P NMR ; 2D NMR ; Chiral discrimination ; Aromatic ring current ; Molecular structure ; MOPAC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis of a novel chiral discriminating reagent, the ester resulting from the reaction of L-menthylphenylphosphoryl chloride with ethanol, is reported. This reagent, C, is aimed to differentiate the R and S monodeuterated enantiomers of ethanol, which constitutes an important isotopic probe for mechanistic studies and origin inference of natural products. The proportions of the two P-epimeric structures, CA and CB, which compose reagent C are directly accessible by 31P NMR. Analysis of 1D and 2D NMR spectra and theoretical simulations enable the 1H and 13C chemical shifts of CA and CB to be determined. The chemical shift differences exhibited by the methylenic hydrogens of the ethoxy moiety in CA and CB are of the order of 0.3 ppm. These large differences can be mainly attributed to ring current effects. Such effects have been estimated using two different methods on the basis of model conformations of the two epimers, CA and CB, deduced from energy minimization in a quantum mechanical approach. The relative signs of the chemical shift differences δR(C) - δS(C) associated with the pro-R and pro-S positions in the CA and CB isomers cannot be determined from the proton spectrum. The ring current calculations suggest that δR(C) - δS(C) are of opposite signs in the two P-epimers. This interpretation, and consequently the conformational analysis, are supported by the 2H NMR study of a chiral discriminating ester prepared from ethanol selectively enriched in deuterium in the pro-R position by stereospecific exchange reactions involving the enzymatic pair alcohol dehydrogenase-diaphorase. The chiral discriminating reagent, C, was then used for determining the enantiomeric imbalance in ethanol samples obtained from biosynthesis under different conditions, and site-specific fractionation factors were calculated.
    Additional Material: 4 Ill.
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  • 10
    ISSN: 0749-1581
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 2-Dimethoxyphosphoryl-1,3-dithiane was obtained by the reaction of 2-chloro-1,3-dithiane with trimethyl phosphite. Studies at 200, 360 and 400 MHz using 1H, 13C and 31P nuclei and 1D- and 2D NMR techniques are described. Long-range coupling constants were extracted by iterative treatment of [AB]2CDMR6X spin systems. A rigid dithiane structure with axial phosphorus is consistent with the NMR results. Analogous dithianes and solid-state structures are discussed.
    Additional Material: 2 Ill.
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