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  • Chemistry  (91)
  • General Chemistry  (38)
  • Industrial Chemistry  (4)
  • 1
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Journal für Praktische Chemie/Chemiker-Zeitung 337 (1995), S. 472-477 
    ISSN: 0941-1216
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Amino-thieno[2,3-c]pyrazoles and Amino-thieno[2,3-b]pyrrolesThe synthesis of thieno[2,3-c]pyrazoles and thieno[2,3-b]pyrroles is described. From the dithioliumsalt (1) and potassium hydroxide the potassium-(2,2-dicyan-1-methylthio-ethen-1-yl)-thiolate (2) is formed. This reacts with hydrazine hydrate to form the 3-amino-5-thioxo-pyrazol-4-carbonitrile (3) S-Alkylation with α-chlorocarbonyl compounds yielding (6a-c) leads via Thorpe-Ziegler-cyclization to 3,4-diamino-thieno[2,3-c]pyrazoles (9) if the position 1 is alkylated (8). Acetyl acetone yields 2-mercapto-pyrazolo[1,5-a]pyrimidine (5). After S-alkylation (10a-d) are immediately cyclized to thieno [2′,3′:3,4]pyrazolo[1,5-a]pyrimidine (11a-d). The ketone (6a) can be cyclized to the pyrazolo [5,1-b]thiazole (12). 3 reacts with oxalyl chloride to form the 2,3-dioxo-6-thioxo-imidazo[1,2-b]pyrazole (13) of which S-phenacyl derivative (14) because the NH-proton cannot be cyclized. The 5-amino-3,4-dicyano-pyrrol-2-thiolate (16) shows the analogous behaviour. The S-alkylation is followed by cyclization, and 3,5-diamino-thieno[2,3-b]pyrroles (18a-b) arise. Reaction of 5-amino-2-alkylthio-pyrrol-3,5-dicarbonitrile (17) with acetyl acetone provides pyrrolo[1,2-a]pyrimidine (20a-c) which can be cyclized to form thieno[3′,2′:4,6]pyrimidines (21a-c) very easily.
    Additional Material: 6 Tab.
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  • 2
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Journal für Praktische Chemie/Chemiker-Zeitung 334 (1992), S. 491-496 
    ISSN: 0941-1216
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: On the Synthesis of 3-Amino-pyrroles by Thorpe-Ziegler-CyclizationN-Aryl and alkylaminomethylene cyanacetic acid derivatives 1 react with α-halogencarbonyl compounds 2 in the presence of potassium carbonate/sodium ethoxide to yield the substituted 3-amino-pyrroles 6. Using the same principle of cyclization pyrrole derivatives 6 can also be obtained by reaction of β-chloro- and β-alkoxymethylenemalononitriles 4 with β-aminocarbonyl compounds 5. From the malononitrile derivatives 1 containing the methylthio group in the β-position, and α-halogen ketones 7, the 2-dicyanomethylene oxazolines 8 arise which undergo alkoholysis by treatment with sodium alkoxide to form the 3-amino-5-alkoxy-pyrrole derivatives 9.
    Additional Material: 3 Tab.
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  • 3
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Journal für Praktische Chemie/Chemiker-Zeitung 338 (1996), S. 206-213 
    ISSN: 0941-1216
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: New Synthesis of Substituted 4-Amino-quinazolines and Their HeteroanalogaN-Chloracetyl-anthranilonitriles react with potassium thiocyanate in the presence of alcohol to the (4-aminoquinazolin-2-yl-thio)-acetic acid ester (5). In the presence of water or primary amine the acetic acid derivative (6) or the acetic acid amide derivatives (7) are obtained. 2,4-Diaminoquinazolines (8) arise if vigorous reaction conditions are employed. With 2-chloracetylamino-cyclopent-1-en-carbonitrile as starting material the pyrimidines (11) are formed from the reaction with potassium thiocyanate. Analogously, (4-pyrimidyl-2-yl-seleno)-acetic acid ester (12) and (thiazolo[4,5-d]pyrimid-2-yl-seleno)-acetic acid derivatives (16) can be prepared with potassium selenocyanate. N-Chloracetyl derivatives of 5-membered heterocycles with enamino-nitrile structure (13, 15, 18, 20) react with potassium thiocyanate to yield thieno[2,3-d]-, thiazolo[4,5-d]-, pyrrolo[2,3-d]-, furo[2,3-d]- and pyrazolo[4,3-d]pyrimidines (14, 16, 19a, 19b, 21).
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Acta Polymerica 43 (1992), S. 335-342 
    ISSN: 0323-7648
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Hydrogele (vernetzte Polymere mit definiertem Wassergehalt) wurden aus hydrophilen Methacrylaten und Perfluorbutylmethacrylat durch radikalische Polymerisation und nachfolgende Quellung in gepufferter isotonischer Natriumchloridlösung hergestellt. Die erhaltenen Hydrogele wurden durch ihre lineare Quellung, den Wassergehalt, den Brechungsindex, den Gehalt an extrahierbaren Bestandteilen, ihre Transparenz für sichtbares Licht sowie durch ihre Sauerstoffpermeation charakterisiert. Derartige Hydrogele sind interessant als Materialien für Kontaktlinsen.
    Notes: Hydrogels (crosslinked polymers with a defined content of water) from hydrophilic methacrylates and perfluorobutyl methacrylate were prepared by radical polymerization, followed by swelling in buffered isotonic sodium chloride solution. The obtained hydrogel samples have been characterized by their linear expansion to hydration, weight-percent hydration, refractive index, extractables, percent transmission of visible light, and oxygen permeability. Such hydrogels are interesting as contact lens materials.
    Additional Material: 10 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Chemie Ingenieur Technik - CIT 38 (1966), S. 994-995 
    ISSN: 0009-286X
    Keywords: Chemistry ; Industrial Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Additional Material: 1 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 406 (1974), S. 167-170 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of LiAl[P(CH3)2]4 and Silylphosphines H3-x(CH3)xSi—P(CH3)2By metallation of HP(CH3)2 with LiC4H9 (in diglyme, at -40°C) and the subsequent reaction of the LiP(CH3)2 with AlCl3 the compound LiAl[P(CH3)2]4 is obtained (solution in diglyme). The reactions with H3SiBr, CH3SiH2Br, (CH3(2)SiHBr, and (CH3)3)SiCl results in the formation of H3SiP(CH3)2, CH3SiH2,—P(CH32, (CH3)2)SiHP(CH3)2, and (CH3)3Si—P(CH3)2 in large quantities.
    Notes: Durch Metallierung von HP(CH3)2 mit LiC4H9 in Diglym bei -40°C und anschließende Umsetzung des gebildeten LiP(CH3)2 mit AlCl3 wird das LiAl[P(CH3)2]4 zugänglich (Lösung in Diglym). Die Umsetzung mit H3SiBr, CH3SiH2Br, (CH3)2SiHBr und (CH3)3SiCl führt zur präparativen Darstellung von H3Si—P(CH3)2, CH3SiH2—P(CH3)2, (CH3)2SiH—P(CH3)2 (CH3)3Si—P(CH3)2.
    Additional Material: 1 Ill.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 407 (1974), S. 295-304 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of Silylphosphines of the X3-(n+m)(CH3)nHmSi—PH2 Type (X = F, Cl, Br)Reactions of halosilanes with silylphosphines containing PH2-groups are reported. CH3SiHCl—PH2 is obtained by (1) For the synthesis of Cl3Si—PH2 reactions of SiCl4 with CH3SiH(PH2)2, CH3SiH2—PH2 and (CH3)3Si—PH2 are carried out in a manner analogous to that shown in eq. (2) Side reactions are observed. Cl3Si—PH2 is isolated in mixture with SiCl4 and CH3SiHCl—PH2 when the most reactive of the above compounds, CH3SiH(PH2)2 is utilized.
    Notes: Es wird über Reaktionen zwischen Halogensilanen und PH2-haltigen Silylphosphinen berichtet. CH3SiHCl—PH2 wird nach Gl. (1) zugänglich. Zur Bildung von Cl3Si—PH2 wurden Umsetzungen von SiCl4 mit CH3SiH(PH2)2, CH3SiH2—PH2 und (CH3)3Si—PH2 durchgeführt, wobei Reaktionen entsprechend Gl. (2) eintreten. Es treten Nebenreaktionen auf. Beim reaktionsfähigeren CH3SiH(PH2)2 ist die Isolierung von Cl3Si—PH2 im Gemisch mit SiCl4 und CH3SiHCl—PH2 möglich. Unter den Reaktionsbedingungen (50°C) zerfällt Cl3Si—PH2 in PH3 und Si—P-Polymere. SiBr4 reagiert bereits bei Raumtemperatur. Durch Umsetzung mit CH3SiH(PH2)2 werden je nach Reaktionsdauer CH3SiHBr—PH2, Br3Si—PH2 und auch Br2Si(PH2)2 zugänglich. Auch die Reaktion mit CH3SiH2—PH2 führt zum Br3Si—PH2 neben CH3SiH2Br. Mit FSiBr3 bildet CH3SiH(PH2)2 das FSiBr2—PH2 neben CH3SiHBr—PH2, während bei den F-reicheren Derivaten F2SiBr2 und F3SiBr die Disproportionierung in SiF4 gegenüber der Si—P-Spaltung überwiegt. Es werden die NMR-Daten der Verbindungen angegeben.Cl3Si—PH2 decomposes into PH3 and Si—P-polymers under the reaction conditions (50°C). SiBr4 however will react at room temperature. Depending on the time of reaction CH3SiHBr—PH2, Br3Si—PH2 and even Br2Si(PH2)2 are obtained with CH3SiH(PH2)2. Also the reaction with CH3SiH2—PH2 leads to the formation of Br3Si—PH2 in addition to CH3SiH2Br. With FSiBr3, CH3SiH(PH2)2 forms FSiBr2—PH2 together with CH3SiHBr—PH2. In the reaction of the higher fluorinated derivatives F2SiBr2 and F3SiBr the disproportion into SiF4 is found to be preferred to Si—P cleavage and therefore these reactions can not be adequately used. The nmr data are reported.
    Additional Material: 3 Tab.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 409 (1974), S. 137-151 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: NMR Studies on Silylphosphines. II. Effects of Substituents in Silyl- and SilylmethylphosphinesThe influence of the substituents [CH3, H, H3Si, (CH3)3Si] on: chemical shifts of protons and phosphorus nuclei: the 29Si-31P coupling constant; and several proton coupling constants in the nmr spectra of 24 silylphosphines of the series (CH3)xH3-x,Si-PH2, (CH3)xH3-xSi-PHCH3, (CH3)xH3-xSi-P(CH3)2, [(CH3)xH3-xSi]2PH, [(CH3)xH3-xSi]2PCH3, [(CH3)xH3-x,Si]3P has been studied. Empirical methods for the calculation of δ31P and J29Si-31P using bond increments are reported.
    Notes: Es wird der Einfluß der Substituenten [CH3, H, H3Si, (CH3)3Si] auf die chemische Verschiebung der Protonen und der Phosphorkerne sowie auf die 29Si-31P-Kopplungskonstante und auf einige Protonenkopplungen in 24 Silylphosphinen der Gruppen (CH3)xH3-x,Si-PH2, (CH3)xH3-xSi-PHCH3, (CH3)xH3-xSi-P(CH3)2, [(CH3)xH3-xSi]2PH, [(CH3)xH3-xSi]2PCH3, [(CH3)xH3-x,Si]3P anhand der NMR-Spektren untersucht. Es werden empirische Verfahren zur Berechnung von δ31 und J29Si-31P aus Bindungsinkrementen mitgeteilt.
    Additional Material: 6 Ill.
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 428 (1977), S. 222-224 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The LiPH2 ·1 MonoglymeA convenient synthesis of the crystalline LiPH2 · 1 monoglyme is reported by metallating PH3 with n-butyllithium in monoglyme (86% yield relative to n-butyllithium). LiPH2 · 1 monoglyme is stable at room temperature and reasonably soluble in thf, mono-, di-, and triglyme. On pumping (oil pump) it decomposes to “Li2PH” liberating PH3 and monoglyme. “Li2PH” is insoluble in the above mentioned solvents.
    Notes: Es wird die präparative Darstellung von kristallinem LiPH2 · 1 Monoglym (Monoglym = Äthylenglykoldimethyläther) durch Metallierung von PH3 mit n-Butyl-Lithium in Monoglym beschrieben (Ausbeute 86% bezogen auf Lithiumbutyl).LiPH2 · 1 Monoglym ist bei Raumtemperatur beständig und gut löslich in THF, Monoglym, Diglym und Triglym. Beim Abpumpen (Ölpumpe) geht es unter Abgabe von PH3 und Monoglym in “Li2PH” über, das in den genannten Lösungsmitteln nicht löslich ist.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 552 (1987), S. 50-68 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Transition Metal Phosphido Complexes. XIV. P-Functional Phosphido-Bridged Heterobimetallic Complexes with and without a Metal-Metal Bond; PH2-Bridged cp(CO)xFe-DerivativesCleaving both Si—P bonds in the complexes cp(CO)2[μ-P(SiMe3)2]M′Lm 1 (M′Lm = Co(CO)2(NO) b, Fe(CO)(NO)2 c Mn(NO)3 d, Cr(CO)5 f, Mo(CO)5 g, W(CO)5 h, Mncp(CO)2 i, MnMecp(CO)2 j, Crcp(CO)(NO) k, Vcp(CO)3 l) using CH3OH, H2O or CH3COOH, respectively, gives the PH2-bridged bimetallic complexes cp(CO)2Fe(μ-PH2)M′Lm 2b-d and 2f-l. The complexes H3PM′Lm 4e, 4f, 4j (M′Lm = Fe(CO)4 e) which can be obtained reacting the P-silylated derivatives (Me3Si)3PM′Lm with CH3OH can be transformed into LiH2PM′Lm 5e, 5f, 5j using n-BuLi. 5e, 5f, 5j react with cp(CO)2 FeBr to give 2e, 2f, 2j. The photochemical decarbonylation of 2b-l leads only in the case of 2i and 2j to isolable complexes containing a metal-metal bond cp(CO)Fe(μ-CO, μ-PH2) M′Lm-1 6 (M′Lm-1 = Mncp(CO) i, MnMecp(CO) j). 6i and 6j as well as 6k (M′Lm-1 = Crcp(NO) k) are also available cleaving both Si—P bonds in cp(CO)Fe[μ-CO, μ-P(SiMe3)2]M′Lm-1 8i-k using CH3OH. In other complexes 6 the PH2-bridge causes a labilisation of the metal-metal bond. This can be used in some cases to add ligands under mild conditions. I.R., N.M.R. and mass spectral data are reported.
    Notes: Durch spaltung beider Si—P-Bindungen in den komplexen cp(CO)2Fe[μ-P(SiMe3)2]M′Lm 1 (M′Lm = Co(CO)2(NO) b, Fe(CO)(NO)2 c, Mn(NO)3 d, Cr(CO)5 f, Mo(CO)5 g, W(CO)5 h, Mncp(CO)2 i, MnMecp(CO)2 j, Crcp(CO)(NO) k, Vcp(CO)3 1) mit Ch3OH, H2O bzw. CH3COOH sind die PH2-verbrückten Zweikernkomplexe cp(CO)2Fe(μ-PH2)M′Lm 2b-d und 2f-1 erhältlich. Die Komplexe H3PM′Lm 4e, 4f, 4j, (M′Lm = Fe(CO)4 e), die aus den P-silylierten Derivaten (Me3Si)3PM′Lm 3e, 3f, 3j, durch Umsetzung mit CH3OH zugänglich sind, lassen sich mit n-BuLi in LiH2PM′Lm 5e, 5f, 5j überführen. 5e, 5f, 5j reagieren mit cp (CP)2FeBr zu 2e, 2f, 2j. Die photochemische CO-Abspaltung aus 2b-1 führt nur bei 2i und 2j zu isolierbaren komplexen mit Metall-Metall-Bindung cp(CO)Fe(μ-CO, μ-PH2)M′Lm-1 6 (M′Lm-1 = Mncp(CO) i, MnMecp(CO) j). 6i und 6j sind ebenso wie 6k (M′Lm-1 = Crcp(NO) k) auch durch Spaltung beider Si—P-Bindungen in cp(CO)Fe[μ-CO, μ-P(SiMe3)2]M′Lm-1 8i-k mit CH3OH erhältlich. Bei anderen Komplexen 6 bewirkt die PH2-Brücke eine Labilisierung der Metall-Metall-Bindung. Dies läßt sich in einigen Fällen zur Addition von Liganden unter milden Bedingungen ausnutzen. NMR-und IR-spektroskopische sowie massenspektrometrische Daten werden mitgeteilt.
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