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  • Articles  (44)
  • Chemistry  (43)
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  • 1995-1999  (44)
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  • Articles  (44)
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  • 1
    Electronic Resource
    Electronic Resource
    Reactions at Silicon-Silicon Bonds, V. Selective Trichlorosilylation of Alkyl(diorganylamino)chlorophosphanes with Hexachlorodisilane or with Trichlorosilane/Triethylamine. - Two Routes to New Functional Trichlorosilylphosphanes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 615-619 
    Details
    ISSN: 0009-2940
    Keywords: Reductive silylation ; Aminochlorophosphanes ; Silylphosphanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of alkyl(diorganylamino)chlorophosphanes R(R2′N)PCl 1 (1a: R = tBu, R′ = Et, 1b: R = iPr, R′ = iPr; 1c: R = iPr, R′ = Ph) with hexachlorodisilane, afforded alkyl(diorganylamino)trichlorosilylphosphanes R(R2′N)PSiCl3 2 (2a: R = tBu, R′ = Et; 2b: R = iPr, R′ = iPr; 2c: R = iPr, R′ = Ph) and silicon tetrachloride. An intermediate formed in the reaction of 1b with hexachlorodisilane, the adduct iPr(iPr2N)(Cl)P-Si(Cl)3-SiCl3 (3b = 1b · Si2Cl6), was detected by 31P- and 29Si-NMR spectra that indicate pentacoordinated silicon bound to tetracoordinated phosphorus and tetracoordinated silicon. Trichlorosilylphosphanes 2 are also available from 1 under very mild conditions by reductive trichlorosilylation with trichlorosilane in the presence of triethylamine. Compounds 2 were identified analytically, by mass spectroscopy, multinuclear NMR, and an X-ray structure determination of 2c.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280614
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  • 2
    Electronic Resource
    Electronic Resource
    Reactions of Silicon-Silicon Bonds, VIFor part V, see ref.[1].. Reductive Trichloroslilylation Reactions Leading to Alkyl- and Dialkylaminobis(trichlorosilyl)phosphanesDedicated to Professor Walter Siebert on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 377-384 
    Details
    ISSN: 0009-2940
    Keywords: Trichlorosilylation ; Dichlorophosphanes ; Silylphosphanes ; Amino(silyl)phosphanes ; Silicon /Reductions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reactions of hexachlorodisilane and of trichlorosilane/triethylamine with alkyl-and dialkylaminodichlorophosphanes RPCl2 1a-i [R = iPr: a; (Me3Si)2CH: b; R=1-adamantly: c: R=tBu: d; R=Et2N: e; R=iPr2M: f] furnish bis(trichlorosilyl)-phosphanes RP(SiCl3)2 3a-f. However, when less bulky substituents are attached to the phosphorus atom, so that there is little steric crowding, the double reductive silylations leading from 1 to 3 are accompanied by side reactions and decomposition of 3. Therefore, only 3b, 3c, 3d, and 3f wre isolated in a pure state. These compounds are more readily prepared by the; trichlorosilane/triethylamine method. 1H-, 31P- and 29Si-Nmr spectra confirm their constitution. The structure of solid 3f, the first aminobis(trichlorosilyl)phosphane, was determined by X-ray crystallography. 3f contains a phosphorus atom in a pyramidal environment surrounded by two silicon atoms and a planar nitrogen atom of the diisopropylamino group.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300312
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  • 3
    Electronic Resource
    Electronic Resource
    Reversible Rearrangements of Chlorophosphane-Dichlorogermylene Ylides to Trichlorogermylphosphanes  -  Structure Determination of a Tetranuclear Bis(chlorophosphane)bis(trichlorogermylphosphane) Silver Bromide Complex (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1619-1623 
    Details
    ISSN: 0009-2940
    Keywords: Dichlorogermylene ; Trichlorogermylphosphanes ; Insertion ; Silver bromide complex ; Carbene homologues ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Chlorophosphanes RR'PCl (1a: R,R' = 1b: R = tBu, R' = iPr, 1c: R = iPr, R' = Et2N, 1d: R = Et2N react with the dichlorogermylene dioxane complex 2 furnishing trichlorogermylphosphanes RR'PGeCl3 4a-d. In the cases of 1c/4c and 1d/4d the insertion reaction remain incomplete; similarly, 4a always contains, shortly after isolation in pure state, small amounts of 1a that can be detected by NMR. A provided by the reaction of trichlorosilylphosphane tBu(Et2N)PSiCl3 (5d) with GeCl4. The alkyl(dialkylamino) trichlorogermylphosphane 4d exists only in an equilibrium with chlorophosphane 1d, which coordinates GeCl2 leading to the dichlorogermylene complex 3d. A 1:1 mixture of 4a with 1a is formed by the novel cleavage (“chlorogermylation”) of the P-P bond of tetraisopropyldiphosphane with germanium tetrachloride. Di-tert-butyl(trichlorogermyl)phosphane 4e (R, R' = tBu) reacts with silver bromide providing a crystalline silver complex 7. A structure determination by X-ray diffraction reveals that 7 is [Ag4Br4(tBu2PCl)2(tBu2PGeCl3)2]. 2C7H8. Two of the Ag atoms of the cubane-like (AgBr)4 core of 7 are coordinated by chlorophosphane 1e, the other two by trichlorogermylphosphane 4e.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971301110
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  • 4
    Electronic Resource
    Electronic Resource
    Halogenation of 1-Ethoxy-1-oxophosphindolin-3-one, a Potential Phosphaindigo Precursor (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1765-1770 
    Details
    ISSN: 0009-2940
    Keywords: Phosphinic acid ; Phosphaindole bromination and chlorination ; Layer structure ; Hydrogen bonds ; Bromine-bromine interaction ; Phosphorus heterocycles ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The bromination of 1-ethoxy-1-oxophosphindolin-3-one (1) with two equivalents oi bromine occurs with elimination of hydrogen bromide and ethyl bromide, providing 2,2-di- bromo-1-hydroxy-1-oxophosphindolin-3-one (4) in high yield. In the presence of triethylamine this process leads to 2,2-dibromo-1-ethoxy-1-Oxophosphindolin-3-one (3) instead. Triethylamine deprotonates 4, providing the solid triethylammonium salt 5. Silylation of 4 with chlorotrimethylsilane leads to the trimethylsilyl ester 6. Monobromination in a two-phase reaction allows the isolation of a mixture of isomers of 2-bromo-1-ethoxy-1-oxophosphindolin-3-one (2a, b). Chlorination with chlorine furnishes 2,2-dichloro-1-ethoxy-1-oxo-phosphindolin-3-one (7). The new compounds 2-7 were characterized analytically and spectroscopically (EI-MS, 1H, 13C and 31P NMR). The crystal structure of acid 4 was determined by X-ray diffraction. Solid 4 consists of aryl stacks connected by chains of P—OH…O==P hydrogen bonds and secondary Br…Br contacts.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971301210
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  • 5
    Electronic Resource
    Electronic Resource
    Dichlorogermylene-Alkyldichlorophosphane Reactions Revisited: Characterisation of Bis(trichlorogermyl)phosphanes, Trichlorogermyldiphosphanes, and Ge-P Heterocycles (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1611-1618 
    Details
    ISSN: 0009-2940
    Keywords: Alkyldichlorophosphanes ; Insertions ; Carbene homologues ; Germanium ; Phosphonium germanate(II) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reactions of alkyldichlorophosphanes 1 (RPCl2; R = tert-butyl: 1a, R = isopropyl; 1b, R = 1-adamantyl: 1c) with the germanium dichloride dioxane complex were followed by 31P NMR. Depending on the organic substituents and the reaction conditions, mixtures of trichlorogermylphosphanes RP(GeCl3)2 4a-c, RPHGeCl3 5a-c, diphosphanes R(H)PP(H)GeCl3 6a-c, R(Cl)PP(H)GeCl3 7a, b cyclophosphanes, and Ge-P heterocycles such as triphosphadigermolanes (RP)3(GeCl2)2 8a, b and tetraphosphagermolane (RP)4)GeCl2 10b are formed. As a further unexpected byproduct of the reaction of 1a with GeCl2-dioxane, a small amount of tri-tert-butyl(trichlorogermyl)cyclotetraphosphane 9a was isolated. From the reaction of 1c with two equivalents of GeCl2-dioxane, separation from byproducts 5c and 6c by crystallisation furnished colourless crystals of 4c (R = 1-adamantyl) as the first pure organylbis(trichlorogermyl)phosphane. Surprisingly, the reaction of isoprophylphosphane with germanium tetrachloride, intended to prepare 5a, led to crystalline isopropylphosphonium trichlorogermanate(II) 11. The structures of molecular 4c and 9a and ionic 11 were determined by X-ray crystallography.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971301109
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  • 6
    Electronic Resource
    Electronic Resource
    Synthesis and Characterization of Titanium Complexes Containing Potentially Tridentate Amido-cyclopentadienyl Ligands (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 275-277 
    Details
    ISSN: 0009-2940
    Keywords: Titanium complexes ; Amido-cyclopentadienyl ligand ; Tridentate ligand ; Lewis acidity ; Chelate effect ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two new titanium complexes of the general type Ti(η5:η1-C5H4SiMe2NCH2CH2X)Cl2 (X = NMe2 OMe), containing a tridentate ligand, were prepared by reaction of Ti(η5-C5H4Si—Me2Cl)Cl3 with the lithium amide Li(NHCH2CH2X) (X = NMe2, OMe). The 1H—NMR chemical shifts for the protons of the ethylene link were found to vary considerably as a function of the temperature, indicating the presence of an equilibrium between the tri- and bidentate bonding mode of the ligand. A single-crystal X-ray structural analysis of Ti(η5:η1—C5H4SiMe2NCH2CH2OMe)Cl2 revealed that the methoxy function is not intramolecularly coordinated in the solid state.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290305
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  • 7
    Electronic Resource
    Electronic Resource
    Unusual Ring-Closure Reactions During the Oxidation of 1,1′-Bi(3-methylphosphol-2-ene) with Hexafluoroacetone  -  Formation of a Tricyclic Fluorine-Containing PhosphoraneDedicated to Professor Rudolf Taube on the occasion of hbis 65th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 819-822 
    Details
    ISSN: 0009-2940
    Keywords: Hexafluoroacetone ; Phosphorus, pentacoordinated ; Diphosphane diselenide ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reduction of the isoprene - PCl3 adduct 1 with magnesium powder, or with Si2Cl6, furnished P-chloro-3-methyl-phosphol-2-ene, 2, in satisfactory yield. Further reduction of 2 with Si2Cl6 gave the new trichlorosilyl-3-methylphosphol-2-ene, 3. The reaction of 2 with magnesium powder, with 3, or with 1/2 equivalent of Si2Cl6 provided the new γ3P-γP-diphosphane 1,1′-bi(3-methylphosphol-2-ene) 4. Reduction of 4 with Si2Cl6 led to 3. Oxidation of 4 with selenium gave the 1,2-diphosphane diselenide, 5. The oxidation of 4 with hexafluoroacetone led to a mixture of products, from which a novel tricyclic phosphorane 6 was separated. the structure of 196 was determined by X-ray diffraction; the coordination geometry at phosphorus in distorted trigonal bipyramidal, with a very long equatorial P - C(CF3)2 bond of 193.2(2) pm.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300623
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  • 8
    Electronic Resource
    Electronic Resource
    Synthesis of catalytically active polymer-bound Schiff base manganese complexes for selective epoxidation of unfunctionalized olefins (1997)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 35 (1997), S. 3249-3254 
    Details
    ISSN: 0887-624X
    Keywords: unsymmetric Schiff base monomer ; linear polymeric Schiff base complexes ; polymeric catalyst ; unfunctionalized olefins ; epoxidation ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A polymerizable unsymmetric tetradentate Schiff base with one vinyl group 3 was synthesized and copolymerized with styrene in toluene. Mn(III) ion was quantitatively incorporated into the copolymers by the functional moieties. The resulting linear polymer-bound manganese complexes (4a′ and 4b′) were used as catalyst under homogeneous condition for selective epoxidation of unfunctionalized olefins (i.e. styrene, α-methylstyrene and cyclohexene) at room temperature in the presence of iodosylbenzene (PhIO) as the terminal oxidant. The efficacy of epoxidation using the polymeric catalysts was comparable to that of the monomolecular analog. © 1997 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 35: 3249-3254, 1997
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  • 9
    Electronic Resource
    Electronic Resource
    Vinyl monomers bearing chromophore moieties and their polymers. V. Synthesis and fluorescence behavior of a vinyloxy monomer bearing electron-accepting chromophore moiety, N-(2-(vinyloxy)ethyl)-1,8-naphthalimide, and its polymer (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1111-1116 
    Details
    ISSN: 0887-624X
    Keywords: N-(2-(vinyloxy)ethyl)-1,8-naphthalimide ; fluorescence structural self-quenching effect ; C60 ; electron donor ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A vinyloxy monomer bearing electron-accepting chromophore, N-(2-(vinyloxy)ethyl)-1,8-naphthalimide (VOENI), was synthesized by reaction of potassium 1,8-naphthalimide with 2-chloroethyl vinyl ether. VOENI can be homopolymerized by cationic initiation and copolymerized with maleic anhydride (MAn) under radical initiation. The fluorescence behaviors of VOENI and its polymers were investigated. It has been found that the fluorescence intensity of the VOENI monomer is much lower than that of its polymers at the same chromophore concentration. This means that a “structural self-quenching effect” (SSQE) has been also observed in the vinyloxy monomer consisting of an electron-accepting chromophore, which has opposite electronic structure in comparison with acrylates bearing electron-donating chromophores as we have reported previously. The SSQE is attributed to the charge-transfer interaction between the electron-accepting chromophore and the electron-donating double bond in the same molecule. The fluorescence quenching of 1,8-naphthalic anhydride and P(VOENI-co-MAn) by ethyl vinyl ether (EVE), dihydrofuran, triethylamine (TEA), etc. evidences that the electron-rich vinyloxy group does act as an important role in the SSQE of VOENI. C60 can also quench the fluorescence of the polymers, and an upward deviation from the linearity of the Stern-Volmer plot was observed showing that C60 acted as a powerful electron donor to quench the fluorescence of the copolymer. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1111-1116, 1998
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  • 10
    Electronic Resource
    Electronic Resource
    Use of a novel autoassociative neural network for nonlinear steady-state data reconciliation (1997)
    Hoboken, NJ : Wiley-Blackwell
    AIChE Journal 43 (1997), S. 1785-1796 
    Details
    ISSN: 0001-1541
    Keywords: Chemistry ; Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A novel autoassociative neural-network-based estimator for nonlinear steady-state data reconciliation was developed, which is a modified autoassociative feedforward neural network. The main difference between them lies in the minimization of an objective function that includes material imbalance terms of flow rates and compositions as well as the traditional least-square prediction term. Accordingly, this neural network, with the material balance-related equations included in the objective criterion, can perform simultaneously the following basic functions necessary for proper steady-state data rectification: (1) eliminate the nonrandom errors, such as the biases and gross erros, from measurements; (2) filter out the random errors from measured data; and (3) estimate the values of unmeasured process variables, provided data redundancy prevails. This novel neural-network-based reconciliation method is demonstrated on a flotation system.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/aic.690430714
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