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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1995-2000 
    ISSN: 0044-2313
    Keywords: 2,6-Diisopropylphenyl-, Amino(fluoro)boranes ; Amino-imino-boranes ; Diazadiboretidines ; Diazasilaboretidines ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The 2,6-Diisopropyl-phenyl Group as a Bulky Substituent in Boron-Nitrogen Compounds. IIFluoro-bis(amino)boranes R′ (Me3Si)N-BF-NHR (R = 2,6-)Me2CH)2C6H3, R′ = Me (Ia), CH2Me (Ib), CHMe2 (Ic), CMe (Id), SiMe3 (Ie), R (If) react with t-butyllithium (molar ratio 1:1) by elimination of HF to give the amino-imino-boranes (IIa - f). The thermal stabilities of the latter depend upon the steric requirement of the substituent R′, IIa - c and IIe dimerize to yield the diazaboretidines IIIa - c and IIIe. IId remains unchanged at 200°C and above, and IIf isomerizes forming the B-Me substituted diazasilaboretidine IVf. If a twofold amount of t-butyllithium is employed, B-CMe3 substituted diazasilaboretidines (Va - f) are the main products. All compounds are characterized by elemental (C, H) analyses and their mass- and n.m.r. (1H, 13C, 15N (in part), 19F, 29Si) spectra. Characteristic i.r.-bands are reported for the amino-imino-boranes (II). An X-ray structure analysis is presented for IVf.
    Notes: Die HF-Eliminierung aus Fluorbis(amino)boranen des Typs R′ (Me3Si)NBFNHR (R = 2,6-)Me2CH)2C6H3, R′ = Me (Ia), CH2Me (Ib), CHMe2 (Ic), CMe3 (Id), SiMe3 (Ie), R (If)) mit t-Butyllithium im Molverhältnis 1:1 führt zu den Amino-imino-boranen (IIa-f), die - abhängig von der Größe des Substituenten R′ - unterschiedliche thermische Stabilität aufweisen. IIa - c und IIe dimerisieren zu den Diazadiboretidinen IIIa - c und IIIe. IId ist bis über 200°C stabil, während sich IIf bei dem Versuch seiner Isolierung zum Bor-Methyl-substituierten Diazasila-boretidin IVf umlagert. Führt man die gleiche Umsetzung mit t-Butyllithium im überschuß (Molverhältnis 1:2) durch, erhält man fast ausschließlich die Bor-t-Butyl-substituierten Diaza-sila-boretidine Va - Vf.Alle Verbindungen sind elementaranalytisch (C, H) und spektroskopisch MS, NMR (1H, 13C, 15N (teilweise), 19F, 29Si) charakterisiert. Charakteristische IR-Banden werden für die Amino-imino-borane (II) angegeben. Eine Röntgenstruktur-analyse wurde von IVf angefertigt.
    Additional Material: 1 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 608 (1992), S. 147-152 
    ISSN: 0044-2313
    Keywords: 2,4,6-Tri-t-butylphenyl-substituted amino-imino boranes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Supermesityl stabilized IminoboranesAmino-iminoboranes R′(SiMe3)N-B≡N-R: IIc (R′ = CHMe2), IId (R′= CMe3) and IIe (R′ = SiMe3) carrying the supermesityl group (R) on the imino nitrogen atoms have been prepared from the corresponding fluorobis(amino)boranes Ic-e by HF-elimination using t-BuLi (IIc, d) or n-lithio-bis(trimethylsilyl)amid (IIe). The Amino-iminoboranes are thermally stable at room temperature. Upon treatment of the fluorobis(amino)boranes Ia, Ib, Ie with t-BuLi, LiF and HN(SiMe3)R′ are eliminated and the B-t-butyl substituted iminoborane III is formed. The compounds are characterized by elementar analyses and spectroscopic data (MS, IR, NMR). An X-ray diffraction study has been performed for II d.
    Notes: Amino-imino-borane R′(SiMe3)N-B≡N-R:IIc (R′ = CHMe2), IId (R′= CMe3) und IIe (R′ = SiMe3) mit R = 2,4,6-Tri-t-butylphenyl- wurden aus den entsprechenden Fluorbis(amino)boranen Ic-e durch HF-Eliminierung mit t-Butyllithium (IIc, IId) bzw. Lithiumbis(trimethylislyl)amid (IIe) erhalten. IIc-e sind thermisch stabil und bei Raumtemperatur unbegrenzt haltbar. Die Umsetzungen der Fluorbis(amino)borane Ia (R′ = Me), Ib(R′ = CH2Me) und Ie (R′ = SiMe3) mit t- Butyllithium führen zur Abspaltung von LiF und HN(SiMe3)R′, wobei sich in allen Fällen des B-t-butyl-substituierte Iminoboran III bildet. Die Verbindungen sind elementaranalytisch und spektroskopisch (MS, IR, NMR) charakterisiert. Eine Röntgenstrukturanalyse wurde von IId durchgeführt.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 560 (1988), S. 18-26 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The 2,6-Diisopropyl-phenyl Group as a Bulky Substituent in Boron-Nitrogen Compounds2,6-Diisopropylaniline (RNH2), the monosilylated derivative (RNH—SiMe3) and its lithium salt (RNLiSiMe3) have been reacted with F3B · OEt2 by variation of the reaction conditions. Products as RNH—BF—NR—BF—NHR, 1, RNH—BF—NHR, 3, Me3SiNR—BF2, 4, and (Me3SiNR)2BF, 5 are thus obtained. Substitution of fluorine atoms in 4 by lithium organyls (R′Li) leads to aminoboranes of the type Me3SiNR—B(F)R′ (R′ = Me, CMe3, C6H5, NHR, N(SiMe3Si)2N), 7a-7e. Thermolysis of 7b gives the diazadiboretidine (—BCMe3—NR—)2, 8. Attempted preparation of the corresponding amino-iminoborane by elimination of Me3SiF and HF from 5 or Me3SiNR—BF—NHR, 7d, yielded the benzoannelated heterocycle 6 and the 1,3-diaza-2-sila-4-bore-tidine 9. The compounds are characterized by analyses and their mass and n.m.r. (1H, 11B, 13C, 15N, 19F, 29Si) spectra.
    Notes: 2,6-Diisopropylanilin (RNH2), dessen monosilyliertes Derivat (RNHSiMe3) bzw. dessen Lithiumsalz (RNLiSiMe3) wurden mit F3B · OEt2 bei unterschiedlichen Reaktionsbedingungen umgesetzt. Dabei erhielt man die Produkte RNH—BF—NR—BF—NHR, 1, RNH—BF—NHR, 3, Me3SiNR—BF2, 4 und (Me3SiNR)2BF, 5. Die Substitution von Fluoratomen in 4 mit Lithiumorganylen (R′Li) führt zu Aminoboranen des Typs Me3SiNR—B(F)R′ (R′ = Me, CMe3, C6H5, NHR, (Me3Si)2N) 7a-7e. Die Thermolyse von 7b führt zum Diazadiboretidin (—BCMe3—NR—)28. Versuche aus 5 und Me3SiNR—BF—NHR, 7d, durch Abspaltung von Me3SiF bzw. HF, das entsprechende Amino-Iminoboran darzustellen, ergaben den Benzo-annelierten Heterocyclus 6 und das 1,3-Diaza-2-sila-4-boretidin 9. Die Verbindungen sind analytisch sowie Massen- und NMR- (1H, 11B, 13C, 15N, 19F, 29Si) spektroskopisch charakterisiert.
    Additional Material: 1 Tab.
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  • 4
    Publication Date: 1988-05-01
    Print ISSN: 0044-2313
    Electronic ISSN: 1521-3749
    Topics: Chemistry and Pharmacology
    Published by Wiley
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  • 5
    Publication Date: 1992-02-01
    Print ISSN: 0044-2313
    Electronic ISSN: 1521-3749
    Topics: Chemistry and Pharmacology
    Published by Wiley
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  • 6
    Publication Date: 1995-12-01
    Print ISSN: 0044-2313
    Electronic ISSN: 1521-3749
    Topics: Chemistry and Pharmacology
    Published by Wiley
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