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  • Inorganic Chemistry  (15)
  • 1,1-dichloroethane  (1)
  • 1975-1979  (16)
  • 1
    Electronic Resource
    Electronic Resource
    Heats of solution of 1:1 electrolytes in 1,2- and 1,1-dichloroethane and derived enthalpies and entropies of transfer of electrolytes from water to these solvents (1976)
    Springer
    Journal of solution chemistry 5 (1976), S. 529-542 
    Details
    ISSN: 1572-8927
    Keywords: Electrolytes ; anions ; cations ; heats ; enthalpies ; entropies ; solution ; transfer ; 1,1-dichloroethane ; 1,2-dichloroethane
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Heats of solution of nine electrolytes in 1,2-dichloroethane and of three electrolytes in 1,1-dichloroethane have been determined calorimetrically at various electrolyte concentrations and extrapolated to zero concentration to yield ΔH s o values for these electrolytes. It is shown that values of ΔH t o for transfer from water to the dichloroethanes of 1∶1 electrolytes are often negative, so that these electrolytes can be more stable enthalpically in the less polar solvents. Combinations of the ΔH t o values with previously determined ΔG t o values yield values of ΔS t o for transfer of 1∶1 electrolytes from water to the dichloroethanes. These ΔS t o values are mostly very negative; they can be correlated very well by the method of Abraham, and in this way ΔS t o values for transfer of numerous other anions and cations have been predicted. The Ph4As+/Ph4B− convention yields single-ion entropies of transfer from water to the dichloroethanes in reasonable agreement with values calculated by the correspondence-plot method.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00647376
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  • 2
    Electronic Resource
    Electronic Resource
    Darstellung und Eigenschaften von 3,6-Dihydro-2H-1,4-oxazin-2-onen und 2H-1,4-Oxazin-2-onen (1977)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 110 (1977), S. 3615-3623 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Properties of 3,6-Dihydro-2H-1,4-oxazin-2-ones and 2H-1,4-Oxazin-2-onesCyclization of α-amino acid acetonyl or phenacyl ester hydrobromides 4 yields 3,6-dihydro-2H-1,4-oxazin-2-ones 5, which may be converted into 2H-1,4-oxazin-2-ones 2 by bromination/dehydro-bromination. Upon heating or prolonged standing the 5-methyl derivatives of 5 undergo an unusual disproportionation to yield 6-isopropenyl-2H-1,4-oxazin-2-ones 6 and the corresponding amino acid. Thermolysis of 5e leads to the 2-azabutadiene 9 via cycloelimination of CO2.
    Notes: Cyclisierung von α-Aminosäure-acetonyl(bzw. phenacyl)ester-hydrobromiden 4 ergibt 3,6-Dihydro-2H-1,4-oxazin-2-one 5, die durch Bromierung/Dehydrobromierung in 2H-1,4-Oxazin-2-one 2 übergeführt werden können. 5-Methylderivate von 5 erleiden beim Erhitzen oder bei längerem Stehenlassen eine ungewöhnliche Disproportionierung, bei der 6-Isopropenyl-2H-1,4-oxazin-2-one 6 und die zugrundeliegende Aminosäure gebildet werden. Bei der Thermolyse von 5e entsteht unter Cycloeliminierung von CO2 das 2-Azabutadien 9.
    Additional Material: 4 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19771101115
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  • 3
    Electronic Resource
    Electronic Resource
    Struktur des Silybins, III. Synthese einer 2,3-unsymmetrisch disubstituierten 2,3-Dihydro-1,4-benzodioxin-6-carbonsäure (1977)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 110 (1977), S. 3664-3671 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structure of Silybin, III. Synthesis of a 2,3-Unsymmetrically Disubstituted 2,3-Dihydro-1,4-benzodioxin-6-carboxylic Acidtrans-3-(3,4-Dimethoxyphenyl)-2,3-dihydro-2-(methoxymethyl)-1,4-benzodioxin-6-carboxylic acid (1a) was synthesized by an unambiguous way, and has been proved to be identical with a degradation product previously obtained from dehydrosilybin of natural origin after permethylation and alkali treatment.
    Notes: trans-3-(3,4-Dimethoxyphenyl)-2,3-dihydro-2-(methoxymethyl)-1,4-benzodioxin-6-carbonsäure (1a) wurde auf eindeutigem Wege synthetisiert und erwies sich als identisch mit dem Alkaliabbauprodukt des Dehydrosilybin-pentamethylethers.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19771101120
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  • 4
    Electronic Resource
    Electronic Resource
    2,3,6-Unsymmetrisch substituierte 2,3-Dihydro-1,4-benzodioxine: Stellung des Phenylrestes bei der Synthese nach Vorländer (1977)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 110 (1977), S. 3867-3873 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Condensation of 1-Aryl-1,2-dibromopropane with 4-Substituted Catechols: 2-Position of the Phenyl Substituent in the 2,3,6-Unsymmetrically Substituted 2,3-Dihydro-1,4-benzodioxine MoleculeThe reaction of 4-methyl- and 4-formylcatechol with 1-aryl-1,2-dibromopropane leads to 2,3-trans-2,3,6-trisubstituted 2,3-dihydro-1,4-benzodioxine derivatives with the phenyl substituent in position 2 (1b, 2b). The structure of the reaction products is elucidated by comparing the products with those obtained by an unambiguous synthesis.
    Notes: Bei der Umsetzung von 1-substituiertem 3,4-Dihydroxybenzol mit 1-Aryl-1,2-dibrompropan wurden als einzig kristallisierbare Reaktionsprodukte 2,3-trans-2,3,6-trisubstituierte 2,3-Dihydro-1,4-benzodioxin-Derivate mit dem Phenylsubstituenten in 2-Stellung erhalten (1b, 2b). Die Konstitutionsaufklärung der Reaktionsprodukte erfolgte durch Vergleich mit auf eindeutigem Wege erhaltenen Vergleichssubstanzen.
    Additional Material: 3 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19771101217
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  • 5
    Electronic Resource
    Electronic Resource
    Struktur des Silybins, II. Synthese des Dehydrosilybin-pentamethyläthers und verwandter Verbindungen (1975)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 108 (1975), S. 1482-1501 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structure of Silybin, II. Synthesis of Dehydrosilybin Pentamethyl Ether and Related CompoundsThe overall structure of silybin, the first flavanolignan, has been settled by synthesis of the two possible isomers for dehydrosilybin tetramethyl ether (37 and 46) and of the two possible isomers of dehydrosilybin pentamethyl ether (26 and 27). The identity of one series of the synthetic compounds, namely 26 and 46, with the product derived from natural sources is clearly shown by i.r., n. m. r., and mass spectra. The substance 26 has the systematic name 2-[3t-(3,4-dimethoxyphenyl)-2r-methoxymethyl-1,4-benzodioxan-6-yl]-3,5,7-trimethoxy-4H-chromen-4-one.
    Notes: Je zwei mögliche Isomere des Dehydrosilybin-pentamethyläthers (26 und 27) und des Dehydrosilybin-tetramethyläthers (37 und 46) wurden auf eindeutigem Wege synthetisiert. Dehydrosilybin-pentamethyläther, dargestellt aus natürlichem Silybin, erwies sich als identisch mit synthetisiertem 2-[3t-(3,4-Dimethoxyphenyl)-2r-methoxymethyl-1,4-benzodioxan-6-yl]-3,5,7-trimethoxy-4H-chromen-4-on (26) durch Vergleich der IR-, NMR- und Massenspektren. Damit ist die Konstitution des Silybins, des ersten Vertreters der Flavanolignane, geklärt.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19751080517
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  • 6
    Electronic Resource
    Electronic Resource
    Ein 5-Acetoxy-6-methoxykawain aus Piper sanctum und Synthese beider Diastereomeren (1976)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 109 (1976), S. 1617-1624 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A 5-Acetoxy-6-methoxykawain from Piper sanctum and Synthesis of Both DiastereoisomersThe structural formula 1 has been assigned to a new kawain derivative isolated from the roots of Piper sanctum. The question of relative stereochemistry was solved by a study of the chemical reactions and spectra of the synthetic diastereoisomers 2c and 3c. The c. d. curve showed that 1 was the dextrorotary (5S, 6S)-(+)-enantiomer of the synthetic rel-(5S,6S)-(±)-5-acetoxy-4,6-dimethoxy-6-trans-styryl-5,6-dihydro-2H-pyran-2-one (2c).
    Notes: Aus der Wurzel von Piper sanctum wurde ein weiteres Kawainderivat mit der Konstitution und Konfiguration 1 isoliert. Die Ermittlung der relativen Konfiguration basiert auf dem chemischen Verhalten und den Spektren der beiden synthetisierten Epimeren 2c und 3c. In Verbindung mit den CD-Werten ergibt sich, daß 1 das rechtsdrehende (5S, 6S)-(+)0-Enantionmere des synthetisierten rel-(5S,6S)-(±)-5-Acetoxy-4,6-dimethoxy-6-trans-styryl-5,6-dihydro-2H-pyran-2-ons (2c) darstellt.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19761090503
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  • 7
    Electronic Resource
    Electronic Resource
    1,6-Anhydrofuranosen, IX. Selektive Monotosylierung der 1,6-Anhydro-α-D-galactofuranose. Synthese und Bestimmung der Molekülstruktur der 1,6 :3,5-Dianhydro - α-D-gulofuranose (1979)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 112 (1979), S. 2068-2078 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 1,6-Anhydrofuranoses, IX. Selective Monotosylation of 1,6-Anhydro-α-D-galactofuranose. Synthesis and Structure Determination of 1,6: 3,5-Dianhydro-α-D-gulofuranoseReaction of 1,6-anhydro-α-D-galactofuranose (1a) with 1.7 mol ρ-toluenesulfonyl chloride gives a mixture of all possible tosylates, the 3-0-derivative 1f with than 40% isolated yield predominating. Cyclization of 1f yields 1,6:3,5-dianhydro-α-D-gulofuranose (2a) with 2,5,7-trioxatricyclo[4.2.1.03.8]nonane skeleton. the structure of it being determined by X-ray crystallography and discussed in comparison to the equally determind structure of 1,6-anhydro-α-L-gulofuranose (3a).
    Notes: Umsetzung von 1,6-Anhydro-α-D-galactofuranose (1a) mit 1.7 mol ρ-Toluolsulfonylchlorid liefert ein Gemisch aller denkbaren Tosylate, in dem das 3-0-Derivat 1fmit über 40% isolierter Ausbeute überwiegt. Dieses läßt sich zur 1,6:3,5-Dianhydro-α-D-gulofuranose (2a) mit 2,5,7-Trioxatricyclo[4.2.1.03.8] nonan-Gerüst cyclisieren, deren Struktur wie die der 1,6-Anhydro-α-L-gulofuranose (3a) durch Röntgenstrukturanalyse bestimmt und diskutiert wird.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19791120617
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  • 8
    Electronic Resource
    Electronic Resource
    1,6-Anhydrofuranosen, X. Eine einfache Synthese für 1,6-Anhydro-3-desoxy-α-D-xylo-hexofuranose (1979)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 112 (1979), S. 2337-2341 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1,6-Anhydrofuranoses, X. A Simple Synthesis for 1,6-Anhydro-3-deoxy-α-D-xylo-hexofuranoseTreatment of 1,6-anhydro-2,3,5-tri-O-tosyl-α-D-galactofuranose (1) with KOH in dioxane/water gives by way of cis-elimination 1,6-anhydro-3deoxy-5-O-tosyl-α-D-threo-hexofuranos-2-ulose (2) in good yield, which tends to dimerize easily in an aldol type reaction to 3. NaBH4 reduces 2 stereoselectively to 4a Removal of the tosyl group giving the title compound 4c is accomplished by sodium amalgam.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19791120641
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  • 9
    Electronic Resource
    Electronic Resource
    α-Aminosäuren als nucleophile Acyläquivalente, II. Synthese von γ-Diketonen unter Verwendung von Oxazolin-5-onen (1979)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 112 (1979), S. 3221-3236 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: α-Amino Acids as Nucleophilic Acyl Equivalents, II. Synthesis of γ-Diketones by means of Oxazolin-5-onesOxazolin-5-ones 1, easily obtainable from α-amino acids, undergo base catalyzed addition of acylacetylenes to give 4-(3-oxopropenyl)-derivatives 2, which are cleaved on warming with oxalic acid dihydrate in acetic acid to yield γ-diketones 3. Starting from 4-alkylideneoxazolin-5-ones 7 4 1-branched oxazolinones 8 may be obtained via addition of lithium phenylthio(alkyl)cuprates. Despite of their high sterical hindrance the oxazolinones 8 are converted into α,α-disubstituted γ-diketones 10 as described for 1. The stereochemistry of the base catalyzed addition of benzoylacetylene to 1b has been investigated.
    Notes: Die aus α-Aminosäuren leicht Oxazolin-5-one, 1. addieren basenkatalysiert Acylacetylene zu 4-(3-Oxopropenyl)-Derivaten 2, die sich durch Erwärmen mit Oxalsäure-dihydrat in Essigsäure zu den γ-Diketonen 3 spalten lassen. Ausgehend von 4-Alkylidenoxazolin-5-onen 7 können durch 1,4-Addition von Lithium-phenylthio(alkyl)cupraten 4 1 -verzweigte Oxazolinone 8 erhalten werden, die trotz großer sterischer Hinderung auf analoge Weise in α, α-dialkylverzweigte γ-Diketone 10 überführbar sind. Die Stereochemie der basenkatalysierten Addition von Benzoyllacetylen an 1b wird untersucht.
    Additional Material: 9 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19791120919
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  • 10
    Electronic Resource
    Electronic Resource
    Die Struktur des festen Stickstofftrichlorids (-125°C) (1975)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 413 (1975), S. 61-71 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Structure of Solid Nitrogentrichloride (-125°C)NCl3 crystallizes in the orthorhombic centrosymmetric space group Pnma. The unit cell with the dimensions a = 7.48 ± 0.02, b = 9.35 ± 0,01 and c = 16.48 ± 0,02 Å contains 12 formula units NCl3. The crystal structure at about -125°C was solved by direct methods, using three-dimensional data collected on WEISSENBERG photographs. The structure was refined to a R index of 9.1%. Besides dipol-dipol-forces there are weak N≡Cl and Cl≡Cl interactions determining the crystal structure built up by NCl3-molecules. The average bond length N—Cl is 1.75 ± 0.01 Å, the average angle Cl—N—Cl is 106.8 ± 2°.
    Notes: NCl3 kristallisiert rhombisch in der zentrosymmetrischen Raumgruppe Pnma. Die Elementarzelle mit den Abmessungen a = 7,48 ± 0,02, b = 9,35 ± 0,01 und c = 16,48 ± 0,02 Å enthält 12 Formeleinheiten NCl3. Die Kristallstruktur bei etwa -125°C wurde unter Verwendung von dreidimensionalen WEISSENBERG-Filmdaten mit direkten Methoden aufgeklärt und bis zu einem R-Wert von 9,1% verfeinert. Neben Dipol-Dipol-Kräften spielen schwache intermolekulare Wechselwirkungen über N≡Cl- und Cl≡Cl-Kontakte eine Rolle beim Aufbau der Kristallstruktur aus NCl3-Molekülen. Der gemittelte N—Cl-Bindungsabstand beträgt 1,75 ± 0,01 Å, der mittlere Bindungswinkel ist 106,8 ± 2°.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19754130108
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