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Bis(trimethylsilyl)aminosubstituierte Silane - Synthese und spektroskopische Untersuchungen (1991)

Popowski, E. ; Kosse, P. ; Kelling, H. ; [et al.]

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 594 (1991), S. 179-190

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ISSN: 0044-2313

Keywords: Silanes ; bis(trimethylsily1)amino-substituted silanes ; syntheses ; i. r., 1H, 29Si n.m.r. data ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: Bis(trimethylsilylamino)-substituted Silanes - Syntheses and Spectroscopic InvestigationsThe bis(trimethylsilyl)aminosubstituted silanes Me3-n[(Me3Si)2N]nSiH (n = 1, 2), Me[(Me3Si)2N]ClSiH, and [(Me3Si)2N]3-nClnSiH (n = 1, 2) were obtained by the reaction of the amides (Me3Si)2NLi with the chlorosilanes Me3-nClnSiH (n = 1-3). In the reaction of the amides (Me3Si)2NLi with Cl3SiH in the molar ratio 3:1 [(Me3Si)2N]2ClSiH is formed only. [(Me3Si)2N]3SiH was prepared by interaction of the lithium silylamides [(Me3Si)2N](Me3SiNLi)2SiH with Me3SiCl. The reaction of the lithium silylamides Me(Me3SiNLi)2SiH with Me3SiCl gave the substitution product Me[(Me3Si)2N]2SiH and the cyclodisilazanes (I: R = R′ = Me3SiNH; II: R = Me3SiNH, R′ = (Me3Si)2N).The i.r., 1H n.m.r., and some 29Si n.m.r. data of the compounds are given. The frequencies of the Si-H stretching vibration, the 29Si—1H coupling constants, and the 29Si n.m.r. chemical shifts of the Si(H) signals of the silanes Me3-n[(Me3Si)2N]nSiH (n=1-3) depend on the number of bis (trimethylsily1)amino substituents. For some silanes a splitting of the v(SiH) band was found. This is assumed to be due t o the existence of rotational isomers. Rotational isomeres are indicated by 29Si and 13C n.m.r. spectra for [(Me3Si)2N]3SiH.

Notes: Durch Reaktion von (Me3Si)2NLi mit den Chlorsilanen Me3-nClnSiH (n = 1-3) wurden die bis(trimethylsilyl)aminosubstituierten Silane Me3-n[(Me3Si)2N]nSiH (n=1, 2), Me[(Me3Si)2N]ClSiH und [(Me3Si)2N]3-nClnSiH (n = 1, 2) erhalten. Bei der Umsetzung von (Me3Si)2NLi mit Cl3SiH im Molverhältnis 3:1 entstand nur [(Me3Si)2N]2ClSiH. [(Me3Si)2N]3SiH wurde durch Reaktion des Lithiumsilylamides Me(Me3SiNLi)2SiH mit Me3SiCl dargestellt. Die Reaktion des Lithiumsilylamides Me(Me3SiNLi)2SiH mit Me3SiCl ergab das Substitutionsprodukt Me[(Me3Si)2N]2SiH und die Cyclodisilazane (I: R = R′ = Me3SiNH; II: R = Me3SiNH, R′ = (Me3Si)2N).Die IR-, 1H-NMR- und teilweise die 29Si-NMR-Daten der Verbindungen sind angegeben. Die Bandenlagen der Si—H-Valenzschwingungen, die 29Si—1H-Kopplungskonstanten und die 29Si-NMR-chemischen Verschiebungen des Si(H)-Signals der Silane Me3-n[(Me3Si)2N]nSiH (n = 1-3) sind von der Anzahl der Bis(trimethylsilyl)aminosubstituenten abhängig.In einigen Silanen wurde eine Aufspaltung der v(SiH)-Bande gefunden. Als Ursache wird das Vorliegen von Rotationsisomeren angenommen. Für das Silan [(Me3Si)2N]3SiH zeigten auch 29Si-und 13C-NMR-spektroskopische Messungen Rotationsisomere an.

Additional Material: 4 Tab.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/zaac.19915940121

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Zum Reaktionsverhalten lithiierter Aminosilane RR′ Si(H)N(Li)SiMe3 (1992)

Kosse, P. ; Popowski, E.

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 613 (1992), S. 137-148

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ISSN: 0044-2313

Keywords: bis(trimethylsilyl)aminosubstituted silanes ; synthesis ; lithium silylamides ; reaction behaviour ; cyclodisilazanes ; crystal structures ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: The Reaction Behaviour of Lithiated Aminosilanes RR′Si(H)N(Li)SiMe3The bis(trimethylsilyl)aminosubstituted silances RR′Si(H)N(SiMe3)2 11-16 (R,R′ = Me, Me3SiNH, (Me3Si)2N) are obtained by the reaction of the lithium silylamides RR′Si(H)N(Li)SiMe3 1-10 (R,R′ = Me3SiNLi, Me, Me3SiNH, (M3Si)2N) with chlorotrimethylsilane in the polar solvent tetrahydrofurane (THF). In the reaction of the lithium silylamides [(Me3Si)2N]2(Me3SiNLi)SiH 10 with chlorotrimethylsilane in THF the rearranged product 1,1,3-tris[bis(trimethylsilyl)amino]-3-methyl-1,3-disila-butane [(Me3Si)2N]2Si(H)CH2SiMe2N(SiMe3)2 17 is formed. The reaction of the lithium silyamides RR′ Si(H)N(Li)SiMe3 1-3 (1: R = R′ = Me; 2: R = Me, R′ = Me3SiNH; 3: R = Me, R′ = Me3SiNLi) with chlorotrimethylsilane in the nonpolar solvent n-hexane gives the cyclodisilazanes [RR′ Si—NSiMe3]2 18-22 (R = Me, Me3SiNH, (Me3Si)2N; R′ = Me, Me3SiNH, (Me3Si)2N, N(SiMe3)Si · Me(NHSiMe3)2) and trimethylsilane. The lithium silylamides 4,5,6,9,10 (4: R = R′ = Me3SiNH; 5: R = Me3SiNH, R′ = Me3SiNLi; 6: R = R′ = Me3SiNLi; 9: R = (Me3Si)2N, R ′ = Me3SiNLi; 10: R = R′ = (Me3Si)2N) shows with chlorotrimethylsilane in n-hexane no reaction.The crystal structure of 17 and 21 are reported.

Notes: Die bis(trimethylsilyl)aminosubstituierten Silane RR′Si(H)N(SiMe3)2 11-16 (R,R′ = Me, Me3SiNH, (Me3Si)2N) entstehen bei der Umsetzung der Lithiumsilylamide RR′Si(H)N(Li)SiMe3 1-10 (R,R′ = Me3SiNLi, Me, Me3SiNH, (M3Si)2N) mit Chlortrimethylsilan im polaren Lösungsmittel Tetrahydrofuran (THF). Das Lithiumsilylamid [(Me3Si)2N]2(Me3SiNLi) · SiH 10 reagiert mit Chlortrimethylsilan in THF unter Umlagerung zum 1,1,3-Tris[bis(trimethylsilyl)amino]-3-methyl-1,3-disila-butan [(Me3Si)2N]2Si(H)CH2SiMe2N · (SiMe3)2 17. Die Reaktion der Lithiumsilylamide RR′Si(H)N(Li)SiMe3 1-3 (1: R = R′ = Me; 2: R = Me, R′ = Me3SiNH; 3: R = Me, R′ = Me3SiNLi) mit Chlortrimethylsilan im unpolaren Lösungsmittel n-Hexan ergibt die Cyclodisilazane [RR′Si—NSiMe3]218-22 (R = Me, Me3SiNH, (Me3Si)2N; R′ = Me, Me3SiNH, (Me3Si)2N, N(SiMe3)SiMe(NHSiMe3)2) und Trimethylsilan. Die Lithiumsilylamide 4,5,6,9,10 (4: R=R′ = Me3SiNH; 5: R = Me3SiNH, R′ = Me3SiNLi; 6: R = R′ = Me3SiNLi; 9: R = (Me3Si)2N, R′ = Me3SiNLi; 10: R = R′ = (Me3Si)2N) zeigen mit Chlortrimethylsilan in n-Hexan keine Reaktion. Die Kristallstrukturen von 17 und 21 werden angegeben.

Additional Material: 2 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/zaac.19926130125

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Zum Zusammenhang zwischen 1JSiH-Kopplungskonstanten und Substituentenelektronegativitäten in SilanenHerrn Prof. Dr. Dr. h. c. H. G. O. Becker zum 70. Geburtstag gewidmet (1992)

Wolff, R. ; Jancke, H. ; Radeglia, R. ; [et al.]

New York, NY : Wiley-Blackwell

Journal für Praktische Chemie/Chemiker-Zeitung 334 (1992), S. 248-250

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ISSN: 0941-1216

Keywords: Chemistry ; Organic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The Connection between 1JSiH Coupling Constants and Group Electronegativities in SilanesFrom n.m.r. coupling constants in silanes of the type HSiMe3-n(X)n (X = CH2SiMe3, NHSiMe3, N(SiMe3)2, OSiMePhCH2CH3, OSiMePhCH2Cl; n = 0…3) substituent parameters α for the groups X were deduced showing distinct dependencies not only on the atoms directly bonded to the silicon atom but also on the atoms which are separated by two or more bonds from the silicon atom. These parameters supplement an excisting body of substituent parameters. They can be used to predict coupling constants. The good correlation of the parameters α with the electronegativities χ has been used to estimate group electronegativities of the above mentioned groups and, additionally, of the group OSiH3.

Additional Material: 1 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/prac.19923340309

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Untersuchungen zur Umsetzung von [Lithium(trimethylsilyl)amido]-methyl-trimethylsilylamino-silan Me(Me3SiNLi)(Me3SiNH)SiH mit verschiedenen Elektrophilen (1993)

Kosse, P. ; Popowski, E.

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 619 (1993), S. 613-616

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ISSN: 0044-2313

Keywords: synthesis, lithium silylamide, reaction behaviour, cyclodisilazanes ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: Investigations of the Reaction between the [Lithium(trimethylsilyl)amido]-methyl-trimethyl-silylamino-silane Me(Me3SiNLi)(Me3SiNH)SiH and different ElectrophilesThe lithium silylamide Me(Me3SiNLi)(Me3SiNH)SiH 1 reacts with chlorotrimethylsilan in the nonpolar solvent n-hexane to the N-substitution product Me[(Me3Si)2N](Me3SiNH)SiH 2 and to the cyclodisilazane [Me(Me3SiNH)Si - N(SiMe3)]2 3 nearly in same amounts. The reaction of 1 with chlorotrimethylstannane gives besides small amounts of the cyclodisilazane 3 the N-substitution product Me[(Me3Si)(Me3Sn)N](Me3SiNH)SiH 4. By the reaction of 1 with trimethylsilyltriflate the cyclodisilazane 3 is obtained as the main product. Furthermore 2 and the cyclodisilazane 5 are formed. Ethylbromide shows no reaction with 1 under the same conditions.These results indicate the existence of an equilibrium of the lithium silylamide 1, the silanimine Me(Me3SiNH)Si=N(SiMe3) and lithium hydride.

Notes: Das Lithiumsilylamid Me(Me3SiNLi)(Me3SiNH)SiH 1 reagiert mit Chlortrimethylsilan in n-Hexan zu annähernd gleichen Teilen zum N-Substitutionsprodukt Me[(Me3Si)2N](Me3SiNH)SiH 2 und zum Cyclodisilazan [Me(Me3SiNH)Si - N(SiMe3)]2 3. Bei der Umsetzung von 1 mit Chlortrimethylstannan entsteht neben geringen Mengen des Cyclodisilazans 3 das N-Substitutionsprodukt Me[(Me3Si)(Me3Sn)N](Me3SiNH)SiH 4. Setzt man 1 mit Trimethylsilyltriflat um, entsteht als Hauptprodukt das Cyclodisilazan, 3. Weiterhin bilden sich 2 und das Cyclodisilazan 5. Ethylbromid reagiert unter den gleichen Bedingungen nicht mit 1.Diese Ergebnisse sprechen für die Existenz eines Gleichgewichts zwischen dem Lithiumsilylamid 1 einerseits und dem Silanimin Me(Me3SiNH)Si=N(SiMe3) sowie Lithiumhydrid andererseits.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/zaac.19936190330

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