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  • Supramolecular chemistry  (2)
  • (N-(N′,N′,N″,N″-tetramethyl)guanidinyl)substituted Phosphoryl compounds  (1)
  • 1
    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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  • 2
    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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  • 3
    Electronic Resource
    Electronic Resource
    Synthese, Struktur und einige Reaktionen [N-(N′,N′,N″,N″-tetramethyl)-guanidinyl]-substituierter PhosphorylverbindungenProfessor Hans Jürgen Bestmann zum 70, Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 348-354 
    Details
    ISSN: 0044-2313
    Keywords: N′,N′,N″,N″-Tetramethylguanidine ; (N-(N′,N′,N″,N″-tetramethyl)guanidinyl)substituted Phosphoryl compounds ; Phosphorylamides ; BF3 Adduct of Phosphorylamides ; X-Ray Crystal Structure Analysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Structure, and some Reactions of N-(N′,N′,N″,N″-tetramethyl)guanidinyl-substituted Phosphoryl CompoundsThe tetramethylguanidinyl-substituted phosphoryl compounds 1-10 were prepared in the reaction of the appropriate chlorophosphoryl compounds with either N′,N′,N″,N″-tetramethylguanidine (HTMG) or N-trimethylsilyl-(N′,N′,N″,N″-tetramethyl)guanidine (TMSTMG). With methyl iodide 1 reacted with N-alkylation to give the ammonium salt 11. 1 reacted with BF3 · Et2O at both imino nitrogen atoms with formation of the bis-BF3-adduct 12. The X-ray structure determination of phenylphosphonic acid-bis(N′,N′,N″,N″-tetramethylguanidinide) 3 shows shortened PN-bonds and widened PNC-angles, consistent with the partial double bond character of the PN-bond.
    Notes: Die tetramethylguanidinylsubstituierten Phosphorylverbindungen 1-10 wurden durch Umsetzung der entsprechenden Phosphinsäure- und Phosphonsäure-Chloride mit N′,N′,N″,N″-Tetramethylguanidin (HTMG) oder N-Trimethylsilyl-N′,N′,N″,N″-tetramethylguanidin (TMSTMG) dargestellt. Mit Methyliodid reagierte 1 unter einfacher N-Alkylierung zur Ammoniumverbindung 11. Mit BF3 · Et2O reagierte 1 and beiden Iminostickstoffatomen unter Bildung des Bis-BF3-Adduktes 12. Das Phenylphosphonsäure-bis(N′,N′,N″,N″-tetramethyl-guanidinid) 3 wurde einer Einkristall-Röntgenstrukturanalyse unterzogen. Es wurden leicht verkürzte PN-Bindungen und aufgeweitete PNC-Winkel beobachtet. Dies deutet auf partiellen Doppelbindungscharakter der PN-Bindung hin.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220224
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