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1984 (1)
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1Author    HansH. KarschRequires cookie*
 Title    Funktionelle Trimethylphosphinderivate, VIII [1] Phosphoniumsalze, Oxide und Sulfide von Tetraorganodiphosphinomethanen, R2PCH2P(CH3)2  
 Abstract    Tetramethyldiphosphinomethane (CH3)2PCH2(CH3)2 (la) reacts with HCl/ether to form the mono-and bisquaternary salts [(CH3)2PCH2P(H)(CH3)2]C1 (2) and [(CH3)2(H)PCH2P(H)(CH3)2]Cl2 (3), respectively. The system 1 a/HCl, incorporating 1 a/2/3, represents a useful tool for studying the appearance of XnAA'X'n-spin type systems. These compounds are also prototypes for a variety of other mono-or bis-phosphonium salts, which are formed in the reactions of the diphosphines (CH3)2PCH2PR2 (R — CH3, *-C4H9, C6H5) (la-c) with (CH3)2C0 + HC1, CH3I, *-C4H9Br, C6H5C0C1, (CH3)2PC1 and Br(CH2)nBr (n = 1, 2). Heterocycles are not obtained. The dioxide 14 and the disulfide 15 are also described. Some properties and spectroscopic data (IR, 1 H, 31 P and 13 C NMR) of 26 new compounds are reported and briefly discussed. 
  Reference    (Z. Naturforsch. 34b, 31—43 [1979]; eingegangen am 8. September 1978) 
  Published    1979 
  Keywords    Phosphonium Salts, Oxides, Sulfides, NMR 
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 TEI-XML for    default:Reihe_B/34/ZNB-1979-34b-0031.pdf 
 Identifier    ZNB-1979-34b-0031 
 Volume    34 
2Author    H. Schmidbaur, A. MörtlRequires cookie*
 Title    Ein spiro-bicyclisehes Phosphor-ylid und sein korrespondierendes Phosphoniumkation A Spiro-bicyclic Phosphorus Yhde and its Corresponding Phosphonium Cation  
  Reference    Z. Naturforsch. 35b, 990—993 (1980); eingegangen am 19. Mai 1980 
  Published    1980 
  Keywords    Ylides, Phosphorus Ylides, Phosphonium Salts, Spiro-bicyclic Compounds 
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 TEI-XML for    default:Reihe_B/35/ZNB-1980-35b-0990.pdf 
 Identifier    ZNB-1980-35b-0990 
 Volume    35 
3Author    HansH. KarschRequires cookie*
 Title    Funktionelle Trimethylphosphanderivate, XVII [1]  
 Abstract    Methyl-bis(dimethylphosphinomethyl)phosphan, (Me2PCH2)2PMe Functional Derivatives of Trimethylphosphane, XVII [1] Methyl-bis(dimethylphosphinomethyl)phosphane, (Me2PCH2)2PMe (Me 2 PCH2)2PMe (3) is obtained from MePCl 2 (2a) or MeP(OPh) 2 (2b) and LiCH 2 PMe 2 (1). The oxides [Me 2 P(0)CH 2 ] 2 PMe (4) and [Me 2 P(0)CH 2 ] 2 P(0)Me (5), are formed on the reaction with air. Quaternisation with Mel gives the salts [(Me3PCH2)2PMe]l2 (6) and [(Me3PCH2)2PMe2]l3 (12). For comparison, also the isoelectronic (Me3SiCH2)2PMe (7), and (Me3SiCH2)2P 4 Bu (8), are synthesized and transformed to their methylphosphonium salts 10 and 11. WithCH 2 Br 2 , 3 forms the six-membered heterocycle [MeP(CH 2 PMe2)2CH 2 ]Br2 (13 a), which could not be isolated in a pure state, however. 3 may be metalated by LiBu: Li[Me2PCHP(Me)CH2PMe2] (15), is obtained, but a second metalation step could not be observed. The hydrolysis of 12 under unusual mild conditions (H2O or H2O/CH3OH) gives [Me2P(0)CH 2 PMe3]I (16), and [Me 4 P]I (17), as main products. Properties and NMR data of the new compounds are described. 
  Reference    Z. Naturforsch. 37b, 284—291 (1982); eingegangen am 12. Oktober 1981 
  Published    1982 
  Keywords    Triphosphane (PCPCP), Phosphonium Salts, Hydrolysis, NMR Spectra 
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 TEI-XML for    default:Reihe_B/37/ZNB-1982-37b-0284.pdf 
 Identifier    ZNB-1982-37b-0284 
 Volume    37 
4Author    Hubert Schmidbaur, Ulrich Deschler, Dietmar SeyferthRequires cookie*
 Title    Ylide Complexes of Alkali and Earth Alkaline Metals, VI [1] Neutral and Anionic Ferrocenylmethylides and Fluorenylides  
 Abstract    Coordination properties of phosphorus ylides towards electropositive metals are greatly improved in systems, where the carbanionic charge can be delocalized into the aromatic rings of substituents, as illustrated in the title compounds. The ferrocenyl-substituted ylide 2, synthesized from bis(diphenylphosphino)methane and (ferrocenyl)trimethyl-ammonium iodide via the phosphonium salt intermediate 1, is thus easily converted into the alkali complexes 3 a, b on treatment with NaNH2 or KH in tetrahydrofuran, respec-tively. The intensely coloured products are soluble in a number of organic solvents. NMR spectra of these solutions provide evidence for an interaction between alkali cations and the ferrocenyl rings. -From (C6H5)2CH2P(C6H5)2 and ferrocenylmethyl chloride a di-quaternary salt 4 is obtained, which yields a double-ylide mixture 5 a, b on treatment with base. Hydrolysis of tIiis product affords the ylidic phosphine oxide 6. -The reaction of the ylides 7 and 9 (described previously) with NaNHo, KH or barium metal (in liquid ammonia) leads to the (earth) alkali complexes 8a-c and 10a, b, respectively. With the exception of 8c, but similar to 3a, these materials contain tetrahydrofuran solvate molecules. The 23 Na NMR spectrum of 8a and the pronounced quadrupole broadening of the P(III) signals by the alkali cations in the 31 P NMR spectra of 8 a, b allow structural suggestions for the solution state as proposed in the formulae. Further treatment of 10b with KH yields a potassium complex 11, characterized, i.a.. via a corresponding diquaternary 
  Reference    Z. Naturforsch. 37b, 950—956 (1982); eingegangen am 2. März 1982 
  Published    1982 
  Keywords    Ylides, Alkali Complexes, Phosphonium Salts, Phosphonium Ferrocenylmethylides 
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 TEI-XML for    default:Reihe_B/37/ZNB-1982-37b-0950.pdf 
 Identifier    ZNB-1982-37b-0950 
 Volume    37 
5Author    HerbertW. Roesky, SushilK. Mehrotra, Christoph Platte, Djammschid Amirzadeh-Asl, Bernhard RothRequires cookie*
 Title    und die Röntgenstrukturanalyse eines phosphorhaltigen achtgliedrigen SN-Ringes Synthesis of Four-and Eight-Membered Heterocycles Containing Sulfur, Nitrogen and Phosphorus and the X-ray Structure of a Phosphorus-Containing Eight-Membered SN-Ring  
 Abstract    Eight-membered rings of the composition [S02(NR)2PR']2 3a-d with R = CH3, C2H5, and R' = CH3, CßHs, were prepared from substituted sulfamides and dichlorophosphanes in the presence of a tertiary amine. These molecules were characterized on the basis of X H and 31 P NMR investigations and of mass spectra. 3 a reacts with phosphorus penta-chloride to yield the spirocyclic derivative 4 with the phosphorus atom in the center of two four-membered rings. Methyliodide reacts with 3 a and 3 b under opening of the eight-membered ring and formation of phosphonium salts. The structure of 3 b is discussed in detail. 3b crystallizes in the orthorhombic space group Pna2i with a = 12.60(0), b = 13.27(1), c — 12.62(4) A. 
  Reference    Z. Naturforsch. 35b, 1130—1136 (1980); eingegangen am 9. Mai 1980 
  Published    1980 
  Keywords    Cyclic Sulfonyl Derivatives, Phosphonium Salts, Spiro Compounds, X-ray 
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 TEI-XML for    default:Reihe_B/35/ZNB-1980-35b-1130.pdf 
 Identifier    ZNB-1980-35b-1130 
 Volume    35 
6Author    GrahamA. Bowm, Cornelia Dörzbach, H. Ubert SchmidbaurxRequires cookie*
 Title    Ein-und Zweielektronen-Oxidation von Phosphor-Yliden mit Kupfer(II)-SaIzen One-and Tw oelectron Oxidation of Phosphorus Ylides Using Copper(II) Salts  
  Reference    Z. Naturforsch. 39b, 618 (1984); eingegangen am 14. D ezem ber 1983 
  Published    1984 
  Keywords    Oxidative Coupling, Phosphorus Y lides, Phosphonium Salts, Copper(II) O xidation, Bis(phosphonium ) Salts 
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 TEI-XML for    default:Reihe_B/39/ZNB-1984-39b-0618.pdf 
 Identifier    ZNB-1984-39b-0618 
 Volume    39