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  • 1
    Electronic Resource
    Electronic Resource
    Application of the attached proton test technique in 31P NMR spectroscopy (1984)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 22 (1984), S. 376-378 
    Details
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Intensity modulated 31P NMR spectra were obtained using the pulse sequence published by Patt and Shoolery. This attached proton test (APT) technique for signal assignment could be applied to systems with long-range heteronuclear couplings in P—O—C—H fragments. In a model system derived from the alcoholysis of P4S10 the six reaction products were assigned to the six signals in the 31P NMR spectrum.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1270220606
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  • 2
    Electronic Resource
    Electronic Resource
    Regio- und stereospezifische Addition von Diazomethan an Gibberellinsäure: Ein neuer effektiver Weg zu 1,2-MethylengibberellinenHerrn Professor Dr. Dr. h. c. Klaus Schreiber zum 65. Geburtstag gewidmet (1992)
    New York, NY : Wiley-Blackwell
    Journal für Praktische Chemie/Chemiker-Zeitung 334 (1992), S. 227-230 
    Details
    ISSN: 0941-1216
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Regio- and Stereospecific Addition of Diazomethane to Gibberellic Acid: A New Effective Pathway to 1α,2α-MethylenegibberellinsA new pathway to 1α,2α-methylenegibberellines via pyrazoline intermediates is reported. In contrast to the addition of diazomethane to the Δ1-double bond of corresponding enones in the case of 1 “Umpolung” of the regioselectivity with cis-addition from the α-side to give pyrazoline ester 4 is observed. Subsequent photolysis of 4 leads to the 1,2-cyclopropyl derivative 6. The structures of the key compounds 4 and 6 are confirmed especially by n.m.r. and X-Ray analysis.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prac.19923340305
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  • 3
    Electronic Resource
    Electronic Resource
    Partial Synthesis of [1β,2α,17,17-D4] Gibberellin A1Dedicated to Professor Dr. K. Schreiber on the Occasion of his 70th Birthday (1997)
    New York, NY : Wiley-Blackwell
    Journal für Praktische Chemie/Chemiker-Zeitung 339 (1997), S. 448-452 
    Details
    ISSN: 0941-1216
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An efficient route for an alternative synthesis of gibberllin A1 from gibberellin A3 is described. Based on iodolactonisation the method provides access to gibberellin A1 labeled by deuterium with both high incorporation of the isotope and high stereoselectity at the positions 1β and 2α. The additional deuterium labeling at C-17 was introduced via the corresponding 16-norketone resulting in [1β,2α,17,17-D4] gibberellin A1.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prac.19973390178
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  • 4
    Electronic Resource
    Electronic Resource
    NMR-spektroskopische Untersuchungen an 15N-markierten Phenylamidochlorocyclotetraphosphazenen (1983)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 504 (1983), S. 138-146 
    Details
    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 PhenylamidochlorocyclotetraphosphazenesSome endocyclically 15N labelled phenylamidochlorocyclotetraphosphazenes, 15N4P4Cl7NHPh, 6,8-15N4P4Cl6(NHPh)2 and 4,8-15N4P4Cl6(NHPh)2, as well as the corresponding exocyclically 15N labelled compounds N4P4Cl715NHPh, 6,8-N4P4Cl6(15NHPh)2 and 4,8-N4P4Cl6(15NHPh)2 were prepared, and the 31P and 15N NMR spectra were recorded. In the case of the endocyclically labelled compounds it is possible to determine the relative signs of the coupling constants 1JPN by means of spectra simulation. In order to interprete the relatively large coupling constants 3JPN to the exocyclic nitrogen a Karplus diagram was calculated and discussed.
    Notes: Einige endocyclisch 15N-markierte Phenylamidochlorocyclotetraphosphazene, 15N4P4Cl7NHPh, 6,8-15N4P4Cl6(NHPh)2 und 4,8-15N4P4Cl6(NHPh)2, sowie die entsprechenden exocyclisch 15N-markierten Verbindungen N4P4Cl715NHPh, 6,8-N4P4Cl6(15NHPh)2 und 4,8-N4P4Cl6(15NHPh)2 wurden dargestellt und die 31P- und 15N-NMR-Spektren aufgenommen. Für die endocyclisch markierten Verbindungen lassen sich die relativen Vorzeichen der Kopplungskonstanten 1JPN über Spektrensimulationen bestimmen. Zur Erklärung der verhältnismäßig großen Kopplungskonstanten 3JPN zum exocyclischen Stickstoff wurde ein Karplusdiagramm berechnet und diskutiert.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19835040918
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  • 5
    Electronic Resource
    Electronic Resource
    Schwefeldioxid als Ligand und Synthon. II. Synthese und Reaktionen der Trimethylsilyl-methansulfinsäure und ihrer Derivateauszugsweise vorgetragen: IX. Int. Symposium on Organic Sulphur Chemistry, Riga 1980; Chemiedozententagung der DDR, Rostock 1984 [1]. (1985)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 528 (1985), S. 138-146 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Sulfur Dioxide as Ligand and Synthon. II. Synthesis and Reaction of Trimethylsilyl Methane Sulfinic Acid and its DerivativesSynthesis and reaction of trimethylsilyl methane sulfinic acid and its derivatives, of the type Me3SiCH2S(O)—Y (Y = OH, OM, OR, NR2) synthesized by insertion of SO2 and R1NSO, respectively, into Me3SiCH2MgCl are described. The compounds obtained are characterized by means of i.r., 1H, 29Si, and 13C n.m.r. spectroscopy.
    Notes: Synthese und Reaktionen der Trimethylsilylmethansulfinsäure und ihrer Derivate des Typs Me3SiCH2S(O)—Y (Y = OH, OM, OR, NR2), dargestellt durch Insertion von SO2 bzw. R1NSO in Me3SiCH2MgCl, werden beschrieben. Die Charakterisierung der synthetisierten Verbindungen erfolgt mit Hilfe der IR-, 1H-, 29Si- und 13C-NMR-Spektroskopie.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19855280915
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  • 6
    Electronic Resource
    Electronic Resource
    Untersuchungen an Systemen aus Salzen und gemischten Lösungsmitteln. XXXIV. 27Al- und 1H-NMR-spektroskopische Untersuchungen an Lösungen des Systems AlCl3-Wasser-N,N-Dimethyl- formamid (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 558 (1988), S. 231-239 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Studies on Systems of Salts and Mixed Solvents. XXXIV. 27Al and 1H N.M.R. Spectroscopic Investigations of AlCl3-Water-N,N-Dimethylformamide SolutionsAl3+ ions exist in aqueous solutions as well as in DMF solutions in a sixfold coordination; the coordination of DMF exclusively occurs via the oxygen atom. Because of the small shift difference between the pure aqueous and the pure DMF solution at the 27Al n.m.r. spectra no separated signals were found corresponding to the species with mixed coordination. From the changes of the Al chemical shifts and of the linewidths in dependence of the solvent composition a selective solvation process is suggested. At the 1H n.m.r. spectra for the formyl and methyl protons of DMF separated signals appear for the molecules of the first coordination sphere and of the bulk, respectively. From this the number of directly coordinated DMF molecules can be determined. Up to a DMF content of about x = 0.45 DMF is preferentially coordinated, after that a change of selectivity takes place and accordingly water is preferred at the first coordination sphere.
    Notes: Al3+-Ionen werden sowohl in wäßrigen als auch in DMF-Lösungen sechsfach koordiniert, die Koordination des DMF erfolgt über Sauerstoff. Wegen der geringen Verschiebungsdifferenz zwischen der reinen wäßrigen und der reinen DMF-Lösung treten in den 27Al-NMR-Spektren mit gemischtem Lösungsmittel keine getrennten Signale für gemischt-koordinierte Spezies auf. Aus den Änderungen der Al-chemischen Verschiebung und der Halbwertsbreite der Signale in Abhängigkeit von der Lösungsmittelzusammensetzung werden Hinweise auf eine selektive Solvatation erhalten. In den 1H-NMR-Spektren erscheinen für die Formyl- und Methylprotonen des DMF getrennte Signale für die Moleküle in der ersten Koordinationssphäre und die des restlichen Lösungsmittels. Daraus läßt sich die Anzahl der direkt koordinierten DMF-Moleküle ermitteln. Bis zu einem DMF-Gehalt von x s≈ 0,45 wird bevorzugt DMF koordiniert, danach tritt ein Selektivitätswechsel auf, so daß bevorzugt Wasser koordiniert wird.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885580124
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  • 7
    Electronic Resource
    Electronic Resource
    Imidodiphosphorsäuretetraphenylester als Ligand in Fluorokomplexen 2. Fluorokomplexe des Phosphors (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 571 (1989), S. 127-132 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tetraphenyl Imidodiphosphate as Ligand in Fluoro Complexes. 2. Fluoro Complexes of PhosphorusTetraphenyl imidodiphosphate forms with PF5 in acetonitrile one pentafluoro (II) and two tetrafluoro complexes (I, III). The imidodiphosphate is monodentately bonded in the pentafluoro complex and it is bidentately coordinated in the tetrafluoro complexes. The constitution and configuration of the complexes are concluded from 19F and 31P n.m.r. data.
    Notes: Imidodiphosphorsäuretetraphenylester, (PhO)2P(O)NHP(O)(OPh)2, bildet mit PF5 in CH3CN einen Pentafluoro- (II) und zwei Tetrafluorokomplexe (I, III). Im Pentafluorokomplex ist der Ligand einzähnig, in den Tetrafluorokomplexen dagegen zweizähnig koordiniert. Alle Konstitutions- und Konfigurationsaussagen zu den Komplexen basieren auf 19F- und 31P-NMR-Untersuchungen.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895710113
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  • 8
    Electronic Resource
    Electronic Resource
    Zerfall von 1-n-Butylaminocyclohexyl-phosphonsäure-di-n-butylester (Buminafos) in wäßrigem Medium (1991)
    New York, NY : Wiley-Blackwell
    Journal für Praktische Chemie/Chemiker-Zeitung 333 (1991), S. 85-90 
    Details
    ISSN: 0021-8383
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Degradation of n-Butylaminocyclohexyl phosphonic Acid di-n-Butylester (Buminafos) in Aqueous Medium.In aqueous medium, breakdown of Buminafos (1) is connected with total loss of its herbicidal activity. The phosphorus-carbon bond is cleaved and n-butylcyclohexylidene amine (3), cyclohexanone (5), phosphoric acid mono-n-butyl ester (4) (partly as n-butylamine salt), and 1-aminocyclohexyl phosphonic acid di-n-butylester (8) were found as degradation products of carbon-14 labeled Buminafos. Identification was performed by MS, GC/MS, 1H- and 31P-n.m.r. spectroscopy, by detection of phosphorus, and by means of the radioactivity.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prac.19913330118
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