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  • 11
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 326 (1964), S. 288-295 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Deep blue, liquid, and distillable trialkylsilyl-aryl-diazenes, R3Si—N=N—ar, are prepared by oxidation of either doubly metallated N-trialkylsilyl-N'-aryl-hydrazines in etheral solution at - 70° with bromine or of the analogous singly metallated derivatives by oxygen with yields up to 35%. Their isolation is complicated by their high sensitivity to heterolytic reagents and by the difficulties of separation from by-products. They could be obtained only in 40-85% purity.
    Notes: Tiefblau gefärbte, flüssige und destillierbare Trialkylsilyl-aryl-diazene R3Si—N=N=;ar bilden sich durch Oxydation von zweifach metallierten N-Trialkylsilyl-N'-aryl-hydrazinen in ätherischer Lösung bei - 70° mit Br2 (Rk. 5) oder aus deren einfach metallierten Derivaten mit Sauerstoff nach Rk. (6) mit Ausbeuten bis zu 35%. Ihre Isolierung ist infolge hoher Empfindlichkeit gegenüber heterolytischen Reagenzien und hartnäckigen Anhaftens von Nebenprodukten erschwert; sie konnten nur in Reinheitsgraden von 40-85% angereichert werden.
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  • 12
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 326 (1964), S. 304-308 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Solvolysis, hydrogenation, decomposition on distillation as well as on storage in solution of trialkylsilyl-aryl-diazenes have been studied quantitatively; further reactions with triphenyl methyl, cyclopentadiene, hydroquinone and HgO have been qualitatively examined. Tripropylsilylphenyldiazene was in each case the most stable and the most clearly reacting of the four synthesized blue diazenes.
    Notes: Solvolysen (vgl. Rk. 1), Hydrierungen (vgl. Rk. 4, 5), Selbstzerfall bei der Destillation (vgl. Rk. 6) wie beim Aufbewahren in Lösungen (vgl. Abb. 2) der Trialkylsilyl-aryl-diazene wurden quantitativ verfolgt, einige weitere Reaktionen mit Triphenylmethyl, Cyclopentadien, Hydrochinon und HgO qualitativ erfaßt. Das Tripropylsilylphenyl-diazen erwies sich in jeder Beziehung als das stabilste und auch am eindeutigsten reagierende der vier dargestellten blauen Diazene.
    Additional Material: 2 Ill.
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  • 13
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 326 (1964), S. 296-303 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: It has been shown by examination of ESR, NMR, UV, IR and RRAMAN spectra as well as by analysis, molecular weight determinations, and synthesis that the deep blue, distillable liquid compounds  -  obtained from the oxidation reactions of trialkylsilyl-aryl-hydrazines and their metallated derivatives with O2 or halogens  -  are not free radicals with hydrazyl structure, but trialkylsilyl-aryl-diazenes, R3SiNNR′, together with 10-60% of N-trialkylsilylanilines, R3SiNHR′.
    Notes: Es wird mit Hilfe von ESR-, NMR-, UV-, IR- und RAMAN-Spektren sowie durch Analysen, Molekulargewichtsbestimmungen und Darstellungsreaktionen der Beweis geführt, daß es sich bei den tiefblauen, destillierbaren, flüssigen Substanzen aus den Oxydationen von Trialkylsilyl-aryl-hydrazinen und ihren metallierten Derivaten mit O2 oder Halogen nicht um radikalische Verbindungen mit Hydrazylstruktur, sondern um Trialkylsilyl-aryldiazene R3SiNNR′ handelt, denen 10-60% durch Destillation nicht abtrennbare Trialkylsilylaniline R3SiNHR′ beigemischt sind.
    Additional Material: 6 Ill.
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  • 14
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 326 (1964), S. 309-316 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Bis-[trimethylsilyl]-organyldichlorosilyl-amines, formed by reaction of sodium-bis-[trimethylsilyl]-amide with organyltrichlorosilanes, and their derivatives with phenyl lithium, methanol and ammonia are described
    Notes: Umsetzung von Natrium-bis-[trimethylsilyl]-amid mit Organyltrichlorsilanen führt zu Bis-[trimethylsilyl]-organyldichlorsilyl-aminen, deren Reaktionen mit Phenyllithium, Methanol und Ammoniak beschrieben werden.
    Additional Material: 1 Ill.
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  • 15
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 371 (1969), S. 201-211 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On reaction of alkali metal peroxodisulphates with liquid sulphur trioxide at room temperature the latter is quantitatively reduced to SO2 according to equation (a) in “Inhaltsübersicht”. Peroxodiphosphates react mainly according to (b) and only to an extent of 10 - 15% according to (c). Interaction of potassium peroxodicarbonate and sulphur trioxide is represented to an extent of 60 - 100% by (d) and 40 - 0% by (e), depending on the reaction conditions.
    Notes: Die Umsetzung von Peroxodisulfaten mit flüssigem Schwefeltrioxid bei Zimmertemperatur verläuft quantitativ unter Reduktion des SO3 zu SO2 gemäß Peroxodiphosphate reagieren vorwiegend nach und nur zu 10-15% nach Kaliumperoxodicarbonat setzt sich je nach Reaktionsbedingungen zu 60 - 100% nach (d) und zu 40 - 0% nach (e) um:
    Additional Material: 3 Tab.
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  • 16
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 383 (1971), S. 249-254 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 1,5-Bis(alkylamino)octamethyltrisildiazanes react after metallation with element dichlorides according to reaction 3a and 3b respectivcly by forming ring compounds. In this way 1,2,8-organylsubstituted permethylated cyclotetrasilazanes (I, II) and inorganic eightmembered ringsystems BSi3N4. PSi3N4 and GeSi3N4, were prepared for the first time.
    Notes: 1,5-Bis(alkylamino)oktamethyltrisildiazane reagieren nach Metallierung mit Elementdichloriden über Rk. 3a oder 3 b unter Ringschluß. Neben 1,2,8-organylsubstituierten, permethylierten Cyclotetrasilazancn (I, II) ließen sich so erstmalig anorganische Achtringsysteme BSi3N4. PSi3N4 und GeSi3N4 darstellen.
    Additional Material: 4 Tab.
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  • 17
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 381 (1971), S. 168-175 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Decamethylcyclotetrasilazane (I) was prepared starting with 1,3-dichloropentamethyldisilazane (II), 1.3-dichlorotetramethyldisilazane (III) and 1,3-bis-(methylamino)tetramethyldisilazane (IV). respectively, according to scheme 1, equ. (1), (2) and (3) in the text. (I) does not form, as given in the literature (equ. 4)5, by thermal transformation of bis(methylaminodimethylsilyl)-tetramethylcyclodisilazane (V); in this case exclusively - in equ. (2) and (3) only in side steps - the reaction products are a mixture of N-methylcyclotrisilazanes (scheme 2, VI-IX).
    Notes: Dekamethylcyclotetrasilazan (I) läßt sich aus 1,3-Dichlorpentamethyldisilazan (II), 1,3-Dichlortetramethyldisilazan (III) wie auch aus 1,3-Bis(methylamino)-tetramethyldisilazan (IV) gemäß Schema 1, Rkk. (1) bis (3), nicht jedoch durch die in der Literatur5 beschriebene thermische Umlagerung von Bis(methylaminodimethylsilyl)-tetramethylcyclodisilazan (V) (vgl. Rk. 4) darstellen. Hierbei entsteht ausschließlich, - in den Rkk. (2) und (3) nur auf Nebenwegen -, ein Gemisch von N-Methylcyclotrisilazanen (Schema 2, VI-IX).
    Additional Material: 2 Tab.
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  • 18
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: By reaction of 1.3-dichloro-pentamethyldisilazane and -tetramethyldisiloxane with hydrazine and 1.2-dimethylhydrazine respectively the novel inorganic ring systems (C), (D)/(D′), (E)/(E′) and (F) (see chapter 1) represented by the compounds I-IV could be constructed. So long it was not possible to decide if the compounds of the systems D/D′ and E/E′ have bicyclo[3.3.0]-octane or cyclobutyl-cyclobutane structure.
    Notes: Durch Umsetzung von 1,3-Dichlor-pentamethyldisilazan und -tetramethyldisiloxan mit Hydrazin bzw. 1,2-Dimethylhydrazin ließen sich in den Verbindungen I-IV die neuen anorganischen Ringsysteme (C), (D)/(D′), (E)/(E') und (F) (siehe Kap. 1) aufbauen. Bisher konnte keine endgültige Entscheidung getroffen werden, ob es sich bei den Systemen D/D′ und E/E′ um NSi2N2Si2N- bzw. OSi2N2Si2O-Bicyclo[3,3,0]-oktan- oder um NSi2N—NSi2N- bzw. OSi2N—NSi2O-Cyclobutyl-cyclobutan-Derivate handelt.
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  • 19
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 385 (1971), S. 164-176 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Decachloro-N,N′-bis(silyl)-cyclodisilazane (I), Cl10Si4N2, is formed via the reaction paths of scheme 1. The total substitution of the Cl atoms was achieved by methyllithium (→ II), methanol (→ III), ethanol (→ IV) or methylamine (→ V), whereas dimethylamine only reacted to (VI), and diethylamine to (VII). The stepwise substitution of the Cl atoms was not possible, in this case only mixtures of I with mono-, di- or trisubstituted products were received which gave further dismutation reactions on attempting their isolation. (1) was easily cleaved by HCl, but only (Cl3Si)2NH did result and not, as was hoped, N(SiCl3)3.
    Notes: Dekachlor-N,N′-bis(silyl)-cyclodisilazan (I), Cl10Si4N2, bildete sich auf den Reaktionswegen des Schema 1. Die Totalsubstitution der Cl-Atome gelang mit Methyllithium [→ me10Si4N2 (II)], Methanol [→ (meO)10Si4N2 (III)], Äthanol [→ (etO)10Si4N2 (IV)] oder Methylamin [→ (meNH)10Si4N2 (V)], während mit Dimethylamin nur (me2N)9ClSi4N2 (VI), mit Diäthylamin nur (et2N)6Cl4Si4N2 (VII) entstand. Versuche zur gezielten stufenweisen Substitution der Cl-Atome ergaben weitgehend Gemische des Ausgangsprodukts mit ein-, zwei- oder dreifach substituierten Derivaten, die sich bei Aufarbeitungsversuchen einer Isolierung durch weitere Dismutationen entzogen. Die HCl-Spaltung von I führte nicht wie erhofft zu N(SiCl3)3, sondern nur zu 2 (Cl3Si)2NH.
    Additional Material: 3 Tab.
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  • 20
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 392 (1972), S. 179-187 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Novel inorganic ring systems. XIV. Seven and ninemembered rings with silicon and nitrogen and also with oxygen atomsSynthesis of the novel sevenmembered ring systems Si4N3 and Si4N2O as well as of the ninemembered ring systems Si5N4 and Si5N2O2 was achieved by condensation of α,ω-difunctional building units in high dilution. The single compounds of the novel ring systems are confirmed in their structure by elemental analysis, molar refraction, infrared, nmr and mass spectra. A tenmembered ring system Si4N6 rearranged during its preparation into the Si4N4-cyclotetrasilazane system with two exocyclic amino groups.
    Notes: Durch Kondensation α,ω-difunktioneller Bausteine bei hoher Verdünnung gelang die Darstellung der neuen siebengliedrigen Ringsysteme Si4N3 und Si4N2O sowie der neungliedrigen Ringsysteme Si5N4 und Si5N2O2. Die einzelnen Vertreter der neuen Verbindungsklassen wurden in ihrer Struktur durch Elementaranalysen, Molrefraktionen, IR-, NMR- und Massenspektren bestätigt. Ein zehngliedriges Ringsystem Si4N6 wich dagegen während der Darstellung in das Si4N4-Cyclotetrasilazansystem mit zwei exocyclischen Aminogruppen aus.
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