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  • 1
    Electronic Resource
    Electronic Resource
    Darstellung von phosphor- und fluorhaltigen Calix[4]aren-Derivaten. Konformationsanalyse, Trennung der Konformere und Röntgenstrukturanalyse an einem KonuskonformerHerrn Professor Helmut Werner zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 267-273 
    Details
    ISSN: 0009-2940
    Keywords: Calix[4]arenes ; Supramolecular chemistry ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Preparation of Phosphorus -  and Fluorine-Containing Calix[4]arene Derivatives. Conformational Analysis, Separation of the Conformers, and X-Ray Crystal Structure Analysis of a Cone ConformerHerrn Professor Helmut Werner zum 60. Geburtstag gewidmet.The Calix[4]arene 1 reacts with hexamethyldisilazane or (diethylamino)trimethylsilane to form the bis-trimethylsilyl-ated derivative 2. Treatment of 2 with PF2C1 gives the mono-and bis-difluorophosphites 3 and 4, which react with elimination of Me3SiF or PF3 to yield the monofluorophosphite derivative 5. All four OH hydrogen atoms in 1 are replaced by lithium on reaction with nBuLi with formation of the tetrali-thiated product 6. This has been allowed to react with the Pchlorophosphorinanones 7-9. From 7 the cone conformer 10a is formed, whereas in the case of 8 and 9 a mixture of all four possible conformars 11a-d and 12a-d is obtained. The pure conformers 12a-d are isolated. By refluxing the cone conformer 12a in tetrachloroethane a conformational conversion is effected. In order to evaluate its coordinating ability, 12a was allowed to react with dichloro(cycloocta-1, 5-diene)platinum(II) to form the trans-disubstituted complex 13. In the case of 12a (acetonitrile solvate) a single-crystal X-ray structure analysis has been conducted. The molecule displays a cone conformation, whereby two of the opposing phenyl rings are approximately parallel and the other two approximately perpendicular to each other.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280310
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  • 2
    Electronic Resource
    Electronic Resource
    Synthesis, Structure, and Reactivity of Tetrakis(O,O-phosphorus)-Bridged Calix[4]resorcinols and Their Derivatives (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1715-1720 
    Details
    ISSN: 0009-2940
    Keywords: Calix[4]resorcinols ; Dioxaphosphocins ; Supramolecular chemistry ; Solid-state NMR spectroscopy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis and characterisation of the reactive tetrakis (O,O-phosphorus)-Bridged calix[4]resorcinols 3 and 4 is described. Because of its poor solubility in common organic solvents, a solid-state NMR investigation of 3 (1H, 13C, 31P) was conducted. Reaction of 3 with MeMgl, Me3 SiMNe2, and HNMe2 furnished the η3γ3P-substituted cavitands 5 and 6. Oxidative addition reactions of 6 with the (H2N)2C(=O)/H2O2 (1:1) adduct, tetrachloro-o-benzoquinone (TOB), and hexafluoroacetone (HFA) led to the η4γ5P derivative 7, and to the η5γ5P derivatives 8 and 9. An X-ray crystal-structure determination of the tetrakis(O,O-phosphorus)-bridged calix[4]resorcinol 4 has been conduced. The framework displays the cone conformation; the chlorine atoms are directed inwards.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971301124
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  • 3
    Electronic Resource
    Electronic Resource
    Verbindungen mit dem 1,3-dimethyl-1,3,2-diazaphosphetidin-4-on-Grundgerüst: Synthese von 1,3-Dimethyl-1,3,2-diazaphosphetidin-4-on-2-oxid-Derivaten (1990)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 123 (1990), S. 1307-1312 
    Details
    ISSN: 0009-2940
    Keywords: 1,3,2-Diazaphosphetidin-4-one derivatives ; Urea, phosphorylated ; P-Oxides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Compounds Involving the 1,3-Dimethyl-1.3,2-diazaphosphetidin-4-one Framework Synthesis of 1,3-Dimethyl-1.3,2-diazaphosphetidin-4-one 2-Oxide DerivativesThe oxidation of 1,3,2-diazaphosphetidinones 3, 4, 7-9 to the respective P-oxides using NO2 (3→5 and 4→6) or (Me3SiO)2 (7→10, 8→11, and 9→12) is described. Other diazaphosphetidinone P-oxides 13-15 are obtained by the reaction of N,N′-dimethylurea with phosphonic dichlorides in the presence of triethylamine as an HCl acceptor. The compounds 5, 6, 10 - 15 contain the novel structural element, involving λ4P. The reaction of 10 and 15 with methanol leads to the formation of the acyclic methyl esters MeOP-(=O)(Y)N(Me)C(=O)N(Me)H (20) [Y = N(CH2)4] and (21) [Y = Ph].
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19901230614
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