共查询到20条相似文献,搜索用时 31 毫秒
1.
Dimethyldichlorosilane, 1,2-dichlorotetramethyldisilane, 1,3-dichlorohexamethyltrisilane and methyltris(chlorodimethylsilyl)silane react with diphenylpotassiumphosphide. The resulting bis- and tris(diphenylphosphino)silanes are characterized by IR and29Si as well as31P-NMR-spectroscopy. 相似文献
2.
Arnd-Rüdiger Grimmer Fred von Lampe Mart Mägi Endel Lippmaa 《Monatshefte für Chemie / Chemical Monthly》1984,115(5):561-564
Starting from high-resolution solid-state29Si NMR spectra of two modifications of Y2Si2O7 with different Si-O-Si bond angles it was verified that increasing bond angles cause high-field isotropic29Si chemical shifts. 相似文献
3.
《Journal of organometallic chemistry》1990,399(3):C18-C20
The compounds H2Si[P(SiMe3)2]2 and [H2SiP(SiMe3)2]2 were prepared and characterized by 29Si NMR, 31P NMR, IR and Raman spectroscopy. After thermolysis of these compounds no cyclic silylphosphanes could be detected in the reaction mixture,although this did contain P(SiMe3)3. 相似文献
4.
He Seung Lee Seung-Sock Choi Kyung-Youl Baek Soon Man Hong Eung Chan Lee Jong-Chan Lee Seung Sang Hwang 《European Polymer Journal》2012,48(6):1073-1081
The stereo cyclic siloxane compounds having tetra hydroxyl and tetra methyl group were synthesized by hydrolysis of tetrahydrido tetramethyl cyclosiloxane consisting of four stereoisomers. Among the stereo cyclic isomers, cis-trans-cis tetrahydroxyl tetramethyl cyclosiloxane (2) was separated by recrystallization and was used as a monomer species for preparation of ladder-like polymethylsilsesquioxane (PMSQ). The isolated isomer was directly polymerized in THF with potassium carbonate (K2CO3) by systematic ring condensation. The hydrolyzed stereoisomers were characterized by 1H and 29Si NMR, and HPLC. The structure of the synthesized PMSQs were characterized by size exclusion chromatography (SEC), MALDI-TOF mass, 29Si NMR, and small angle X-ray scattering (SAXS). 相似文献
5.
29Si NMR Investigations on the Anion Structure of Crystalline Tetramethylammoniumaluminosilicates and -aluminosilicate Solutions The 29Si NMR spectra of crystalline tetramethylammonium (TMA) aluminosilicates with different Si/Al ratios exhibit up to 4 sharp signals with characteristic chemical shifts which can be assigned to the central Si atom of OSi(OSi)3?n(OAl)n building units of double four-ring (DFR) aluminosilicate anions. The number and distributions of the Al atoms in the DFR framework can be derived from the signal intensities in connection with the results of the trimethylsilylation method [1]. A good agreement of the results of both methods has been found. The DFR can exist as monomeric unit or can be connected to polymeric structures by SiOAl bridges, but no information can be obtained about this question by the 29Si NMR spectra. The investigation of the TMA aluminosilicate solutions by 29Si NMR and TMS method [1] show that stable aluminosilicate anions exist in these solutions. The structure of these aluminosilicate anions is different from the structure of the crystalline TMA aluminosilicates obtained from the solutions. 相似文献
6.
Die Tris(triisopropylsilyl)pnikogene: Synthese und Charakterisierung von [E(SiiPr3)3] (E = P,As, Sb)
Carsten von Hnisch 《无机化学与普通化学杂志》2001,627(7):1414-1416
The Tris(triisopropylsilyl)pnikogenes: Synthesis and Characterisation of [E(Si i Pr3)3] (E = P, As, Sb) The compounds [E(SiiPr3)3] (E = P, As, Sb) ( 1 – 3 ) were prepared in high yields by the reaction of (Na/K)3E with iPr3SiCl in DME. They were characterised by 1H‐, 13C‐, 29Si‐ and 31P‐NMR spectroscopy, mass spectrometry and single crystal X‐ray diffraction. Compound 1 , recently obtained in a different way, shows an unusual trigonal planar coordination of the central phosphorus atom. However, 2 and 3 , featuring increasing covalence radii of the central atoms, show an increasingly pyramidal structure. 1 – 3 crystallise isotyp in the cubic spacegroup Pa 3, the lattice constants are: 1 : a = 1860.1(2) pm, 2 : a = 1873.6(2) pm, 3 : a = 1897.1(2) pm. 相似文献
7.
Karl Hassler 《Monatshefte für Chemie / Chemical Monthly》1982,113(4):421-425
A simple preparation of the title compounds is achieved by reacting Na3P/K3P with stoichiometric mixtures of chlorotriphenylsilane and chlorotrimethylsilane.31P- and29Si-NMR-Data as well as Ir and Raman spectra of the compounds are reported. 相似文献
8.
A.V Safronova N.E Stolyarova I.K Grigorieva I.P Malysheva G.V Basova G.K Fukin Yu.A Kurskii S.Ya Khorshev G.A Abakumov 《Journal of organometallic chemistry》2004,689(7):1127-1130
The novel organosilicon, -germanium and -tin-containing carbene complexes of tungsten of the type Ph3E-CHWCl2(OBut)2 (E=Si, Ge, Sn) have been prepared by the reaction of heteroelement-containing carbene complexes of tungsten Ph3E-CW(OBut)3 (E=Si, Ge, Sn) with hydrogen chloride. The tin-containing carbene complex was identified in solution by 1H NMR spectroscopy. Silicon- and germanium-containing carbene complexes were isolated in high yields as crystalline solids and characterized by elemental analysis, IR, 1H NMR, 13C NMR and 29Si NMR spectroscopy and X-ray diffraction studies. The geometry of the W atoms in the compounds can be described as a distorted square pyramid. 相似文献
9.
《Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy》1988,44(7):643-646
Silicon-29(δ29Si) NMR chemical shifts are reported for the first time of tris[(trimethylsilyl)methyl] silicon compounds (disilylated derivatives) (Me3SiA)3 CαL, where L = SiBR1R2R3 and where R varies widely in electronegativity. 29Si chemical shifts exhibit good correlation with the electronegativities of the groups bonded to the silicon atom. The 13C NMR spectra of these compounds have been recorded and assigned. δ13Cα is shown to depend on the type of substitutent on SiB. The variation of 29SiH coupling constants with electronegativity of R is studied. 相似文献
10.
M. G. Voronkov E. A. Grebneva O. M. Trofimova A. I. Albanov N. F. Chernov N. N. Chipanina 《Russian Journal of General Chemistry》2006,76(12):1851-1853
Reaction of tetrafluorosilane with tris(2-hydroxyethyl)-and tris(2-trimethylsiloxyethyl)amine results in formation of 1-fluorosilatrane and fluorosilatrane in 75 and 53% yield, respectively. Reaction of tetrafluorosilane with bis(2-trimethylsiloxyethyl)amine and its N-methyl derivative leads to the hitherto unknown 1,1-difluoroquasisilatranes (N → Si) F2Si(OCH2CH2)2NR (R = H, Me) containing donor-acceptor bond N → Si and pentacoordinate silicon atom. The structure of the synthesized compounds was proved by 1H, 13C, 15N, 19F, 29Si NMR and IR spectroscopy. 相似文献
11.
The reaction of trimethylsilyl- and pentafluorophenyl-N-sulfinylamine respectively with 3,5-dihalogeno-1,2,4-trithia-3,5-diborolanes yields the 1,2-dithia-4-aza-3,5-diborolidines1-3.Tert-butyl-N-sulfinylamine and 3,5-dimethyl-1,2,4-trithia-3,5-diborolane react analogous. OtherN-sulfinylamines however split the disulfane bridge in 3,5-dimethyl-1,2,4-trithia-3,5-diborolane and the 1,4-dithia-2-aza-3,5-diborolidines5A-7(A) are formed. Besides of boroxines, cyclo-2,4,6-trimethyl-1,3-dioxa-5-aza-2,4,6-triboranes and cyclo-2,4,6-trimethyl-1-oxa-3,5-diaza-2,4,6-triboranes are formed as byproducts,8–10 have been isolated. In 1,2,4-trithia-3,5-diborolanes and 1,2-dithia-4-aza-3,5-diborolidines the bromo-atoms can be substituted by alkyl (13, 14), by amino (15–20) and by isothiocyanato groups. The compounds were characterised analytically and spectroscopically (MS; NMR:1H,11B,19F,29Si; IR). 相似文献
12.
《Journal of organometallic chemistry》1990,395(2):C23-C25
Triphenylphosphane(2,4,6-tri-t-butylphenylseleno)gold(I) and bis-(2,4,6-tri-t-butylphenylseleno)mercury(II) are obtained from chloro(triphenylphosphane)gold(I) or mercury dichloride with lithium(2,4,6-tri-t-butylphenyl)selenide and with trimethyl(2,4,6-tri-t-butylphenylseleno)silane, respectively. Molecular mass determinations and 1H, 13C and 77Se NMR spectra indicate that both new compounds are monomeric in solution. 相似文献
13.
Syntheses, Single-Crystal X-Ray Analyses and Solid-State 29Si NMR Studies of a Zwitterionic λ5-Spirosilicate and a Cage-like Octa(silasesquioxane) The zwitterionic λ5-spirosilicate bis[2,3-naphthalenediolato(2 ?)][2-(dimethylammonio)phenyl]silicate ( 1 ; isolated as 1 · 1/2 CH3CN) was synthesized by reaction of the [2-(dimethylamino)phenyl]dimethoxyorganosilanes 5, 6 and 7 [2-(Me2N)C6H4Si(OMe)2R: R = Ph ( 5 ), cyclo? C6H11 ( 6 ), Me ( 7 )] with 2,3-dihydroxynaphthalene in acetonitrile at room temperature. Reaction of 1 · 1/2 CH3CN or [2-(dimethylamino)phenyl]trimethoxysilane ( 3 ) with water in acetonitrile yielded the cage-like octa{[2-(dimethylamino)phenyl]silasesquioxane} ( 2 ). The crystal structures of 1 · 1/2 CH3CN and 2 were studied by X-ray diffraction. In addition, 1 · 1/2 CH3CN and 2 were characterized by solid-state (29Si CP/MAS) and solution NMR studies (1H, 13C, 29Si). 相似文献
14.
Preparation, Characterization and Reaction Behaviour of Sodium and Potassium Hydridosilylamides R2(H)Si—N(M)R′ (M = Na, K) — Crystal Structure of [(Me3C)2(H)Si—N(K)SiMe3]2 · THF The alkali metal hydridosilylamides R2(H)Si—N(M)R′ 1a‐Na — 1d—Na and 1a‐K — 1d‐K ( a : R = Me, R′ = CMe3; b : R = Me, R′ = SiMe3; c : R = Me, R′ = Si(H)Me2; d : R = CMe3, R′= SiMe3) have been prepared by reaction of the corresponding hydridosilylamines 1a — 1d with alkali metal M (M = Na, K) in presence of styrene or with alkali metal hydrides MH (M = Na, K). With NaNH2 in toluene Me2(H)Si—NHCMe3 ( 1a ) reacted not under metalation but under nucleophilic substitution of the H(Si) atom to give Me2(NaNH)Si—NHCMe3 ( 5 ). In the reaction of Me2(H)Si—NHSiMe3 ( 1b ) with NaNH2 intoluene a mixture of Me2(NaNH)Si—NHSiMe3 and Me2(H)Si—N(Na)SiMe3 ( 1b‐Na ) was obtained. The hydridosilylamides have been characterized spectroscopically. The spectroscopic data of these amides and of the corresponding lithium derivatives are discussed. The 29Si‐NMR‐chemical shifts and the 29Si—1H coupling constants of homologous alkali metal hydridosilylamides R2(H)Si—N(M)R′ (M = Li, Na, K) are depending on the alkali metal. With increasing of the ionic character of the M—N bond M = K > Na > Li the 29Si‐NMR‐signals are shifted upfield and the 29Si—1H coupling constants except for compounds (Me3C)(H)Si—N(M)SiMe3 are decreased. The reaction behaviour of the amides 1a‐Na — 1c‐Na and 1a‐K — 1c‐K was investigated toward chlorotrimethylsilane in tetrahydrofuran (THF) and in n‐pentane. In THF the amides produced just like the analogous lithium amides the corresponding N‐silylation products Me2(H)Si—N(SiMe3)R′ ( 2a — 2c ) in high yields. The reaction of the sodium amides with chlorotrimethylsilane in nonpolar solvent n‐pentane produced from 1a‐Na the cyclodisilazane [Me2Si—NCMe3]2 ( 8a ), from 1b‐Na and 1‐Na mixtures of cyclodisilazane [Me2Si—NR′]2 ( 8b , 8c ) and N‐silylation product 2b , 2c . In contrast to 1b‐Na and 1c‐Na and to the analogous lithium amides the reaction of 1b‐K and 1c‐K with chlorotrimethylsilane afforded the N‐silylation products Me2(H)Si—N(SiMe3)R′ ( 2b , 2c ) in high yields. The amide [(Me3C)2(H)Si—N(K)SiMe3]2·THF ( 9 ) crystallizes in the space group C2/c with Z = 4. The central part of the molecule is a planar four‐membered K2N2 ring. One potassium atom is coordinated by two nitrogen atoms and the other one by two nitrogen atoms and one oxygen atom. Furthermore K···H(Si) and K···CH3 contacts exist in 9 . The K—N distances in the K2N2 ring differ marginally. 相似文献
15.
Uwe Klingebiel 《Journal of organometallic chemistry》1978,152(1):33-38
Fluorosilanes react with lithiated amines to yield aminofluorosilanes. Iso- and sec-butylaminofluorosilanes with bulky ligands form the isomers (I–VII). The cyclisation of monoorganofluorosilanes depends on the size of the substituents. IV and V dimerise by HF-elimination (VIII, IX) and VII cyclises by migration of a methanide ion (X). The mass, 1H, 19F and 29Si NMR spectra of the compounds are reported. 相似文献
16.
M. G. Voronkov A. I. Albanov E. A. Grebneva O. M. Trofimova N. F. Chernov N. N. Chipanina 《Russian Journal of General Chemistry》2006,76(12):1854-1859
Reaction of phenyltrifluorosilane, diphenyldifluorosilane, and methylphenyldifluorosilane with bis(2-hydroxyethyl)amine, methyl-bis(2-hydroxyethyl)amine, methyl-bis(2-trimethylsiloxyethyl)amine, leads to 1,3-dioxa-6-aza-2-silacyclooctane derivatives, (N → Si) quasisilatranes: 1,1-difluoroquasisilatrane, 1-phenyl-1-fluoro-5-methylquasisilatrane, or 1-methyl-1-fluoroquasisilatrane, containing the donor-acceptor bond N → Si and pentacoordinate silicon atom. 1-Phenylsilatrane was found to be the product of the reaction of phenyltrifluorosilane with tris(2-trimethylsiloxyethyl)amine, whereas with tris(2-hydroxyethyl)amine 1-phenylsilatrane and 1-fluorosilatrane were formed in the molar ratio of 3:1. The structure of the synthesized compounds was proved by 1H, 13C, 15N, 19F, 29Si NMR and IR spectroscopy. 相似文献
17.
Wolfram Uhlig 《Journal of polymer science. Part A, Polymer chemistry》1998,36(5):725-735
Novel poly(silylenemethylenes) have been prepared by the ring-opening polymerization of 1,3-disilacyclobutanes followed by a protodesilylation reaction with triflic acid. The silicon–aryl bond cleavage could be controlled by using different leaving groups, for instance phenyl- and para-anisyl substituents. The reactions of the triflate derivatives with organomagnesium compounds, LiAlH4, amines, or alcohols gave functional substituted poly(silylenemethylenes). Hydrosilylation reactions or reductive coupling with potassium–graphite led to organosilicon network–polymers, which may serve as suitable precursors for silicon carbide and Si/C/N-based materials. The structures of the polymers were identified by NMR spectroscopy (29Si, 13C, 1H). © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 725–735, 1998 相似文献
18.
N‐(trialkoxysilylalkyl) derivatives of 1,2,3,4‐tetrahydroquinoline, 1,2,3,4‐tetrahydroisoquinoline and 4,4‐dimethyl‐4‐sila‐1,2,3,4‐tetrahydroisoquinoline were prepared and characterized by elemental analysis, 1H, 13C and 29Si NMR spectroscopy. In vivo psychotropic properties and in vitro cytotoxic effects of 3‐[N‐(1,2,3,4‐tetrahydroisoquinolyl)]propyltriethoxysilane methiodide and 3‐[N‐(1,2,3,4‐tetrahydroisoquinolyl)]propylsilatrane are reported. Comparative study of 29Si shifts in newly synthesized compounds suggested donor–acceptor interaction between nitrogen and silicon atom, which increased electron density at Si nuclei, revealing a stronger increment of N → Si transannular bond in comparison with N → Si α‐effect. The molecular structure of 3‐[N‐(1,2,3,4‐tetrahydroisoquinolyl)]propylsilatrane features a penta‐coordinate silicon atom having CSiO3 pattern and Si…N intramolecular interaction. Copyright © 2005 John Wiley & Sons, Ltd. 相似文献
19.
David J.T. Hill Christopher M.L. Preston Andrew K. Whittaker Susan M. Hunt 《Macromolecular Symposia》2000,156(1):95-102
The radiation chemistry of poly(dimethyl siloxane) has been investigated with respect to identification of the nature of the small molecule chain scission products. Low molecular weight linear and cyclic products have been identified through the use of 29Si solution NMR, GPC and MALDI‐TOF mass spectrometry. It has been suggested that the low molecular weight cyclic products are formed by back‐biting depolymerization reactions. 相似文献
20.
Synthesis of methylcyclotetra(hexa)siloxanes with different reactive groups at the same silicon atom
N. N. Makarova I. M. Petrova T. V. Vlasova P. V. Petrovskii 《Russian Chemical Bulletin》2006,55(6):968-972
Representatives of methylcyclotetra(hexa)siloxanes with two different reactive groups at the same silicon atom (CH2=CH and Cl, H and Cl, CH2=CH and OH) were synthesized for the first time by condensation of trichlorovinylsilane with dihydroxydimethylsilane, and
by stepwise condensation of trichloro-and trichlorovinylsilane with 1,3-dihydroxy-1,1,3,3-tetramethyldisiloxane in the presence
of amines (aniline, pyridine, and triethylamine). The condensation with 1,3-dihydroxy-1,1,3,3-tetramethyldisiloxane with a
large excess of trichlorosilane, unlike the condensation with trichlorovinylsilane, occured intramolecularly to give monochlorotetramethylcyclotrisiloxane
in a high yield and intermolecularly to give 1,1,7,7-tetrachloro-3,3,5,5-tetramethyl-1,7-dihydrotetrasiloxane. The structures
of the synthesized compounds were confirmed by 1H and 29Si NMR spectroscopy, IR spectroscopy, and mass spectrometry.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 932–936, June, 2006. 相似文献