4142-85-2Relevant articles and documents
Process for Preparing Polysilylalkane
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Paragraph 0045-0047; 0056-0066; 0076-0078, (2020/04/17)
Polysilylalkane according to the present invention is represented by following formula. The present invention has an advantage that bis(silyl)alkanes or tri(silyl)alkanes can be manufactured in a high yield by dehydrochlorination with a small amount of catalyst by using a silane compound having a dichloro organic matter or a dichloromethyl group.COPYRIGHT KIPO 2020
Exhaustively Trichlorosilylated C1 and C2 Building Blocks: Beyond the Müller-Rochow Direct Process
Georg, Isabelle,Teichmann, Julian,Bursch, Markus,Tillmann, Jan,Endeward, Burkhard,Bolte, Michael,Lerner, Hans-Wolfram,Grimme, Stefan,Wagner, Matthias
supporting information, p. 9696 - 9708 (2018/07/21)
The Cl--induced heterolysis of the Si-Si bond in Si2Cl6 generates an [SiCl3]- ion as reactive intermediate. When carried out in the presence of CCl4 or Cl2C=CCl2 (CH2Cl2 solutions, room temperature or below), the reaction furnishes the monocarbanion [C(SiCl3)3]- ([A]- 92%) or the vicinal dianion [(Cl3Si)2C-C(SiCl3)2]2- ([B]2- 85%) in excellent yields. Starting from [B]2-, the tetrasilylethane (Cl3Si)2(H)C-C(H)(SiCl3)2 (H2B) and the tetrasilylethene (Cl3Si)2C=C(SiCl3)2 (B; 96%) are readily available through protonation (CF3SO3H) or oxidation (CuCl2), respectively. Equimolar mixtures of H2B/[B]2- or B/[B]2- quantitatively produce 2 equiv of the monoanion [HB]- or the blue radical anion [B?]-, respectively. Treatment of B with Cl- ions in the presence of CuCl2 furnishes the disilylethyne Cl3SiC≡CSiCl3 (C; 80%); in the presence of [HMe3N]Cl, the trisilylethene (Cl3Si)2C=C(H)SiCl3 (D; 72%) is obtained. Alkyne C undergoes a [4+2]-cycloaddition reaction with 2,3-dimethyl-1,3-butadiene (CH2Cl2, 50 °C, 3d) and thus provides access to 1,2-bis(trichlorosilyl)-4,5-dimethylbenzene (E1; 80%) after oxidation with DDQ. The corresponding 1,2-bis(trichlorosilyl)-3,4,5,6-tetraphenylbenzene (E2; 83%) was prepared from C and 2,3,4,5-tetraphenyl-2,4-cyclopentadien-1-one under CO extrusion at elevated temperatures (CH2Cl2, 180 °C, 4 d). All closed-shell products were characterized by 1H, 13C{1H}, and 29Si NMR spectroscopy; an EPR spectrum of [nBu4N][B?] was recorded. The molecular structures of [nBu4N][A], [nBu4N]2[B], B, E1, and E2 were further confirmed by single-crystal X-ray diffraction. On the basis of detailed experimental investigations, augmented by quantum-chemical calculations, plausible reaction mechanisms for the formation of [A]-, [B]2-, C, and D are postulated.
Process for Preparing Polysilylalkane
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Paragraph 0056; 0058, (2016/11/02)
According to the present invention, polysilylalkane is represented by chemical formula 3. In chemical formula 3, m is equal to n, and n is equal to zero; and R^3 is a chloromethyl group. In the case of R^4 is H, -SiMe_2Cl, -SiMe_3, -SiMeCl_2, and -SiCl_3, R^3 is equal to -SiCl_3. In the case of R^4 is H, and R^5 is equal to R^6 and R^6 is equal to Me, or R^5 is equal to Me and R^6 is equal to Et, R^3 is -SiCl_3. In the case of R^4 is H, R^5 is equal to -CH_2SiCl_3, and R^6 is Me, R^3 is equal to -SiCl_3. In the case of R^4 is H, R^5 is equal to R^6 and R^6 is equal to -CH_2SiCl_3, R^3 is equal to Et, SiMe_2Cl, -SiMeCl_2, and -SiCl_3, and m is an integer of zero to nine. The manufacturing method is capable of manufacturing bis(silyl)alkane or tri(silyl)alkane in a high yield with a small amount of a catalyst.COPYRIGHT KIPO 2016
Process for Preparing Polysilylalkane
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Paragraph 0056; 0057, (2016/10/31)
A polysilyalkane according to the present invention is presented by a formula. Here, m=n=0, R^3 is chloro, and methyl group; when R^4 is H, -SiMe_2Cl, -SiMe_3,-SiMeCl_2, -SiCl_3, R^3=-SiCl_3; R^4 is H, R^5=R^6=Me or R^5=Me, when R6=Et, R^3-SiCl_3; R^4 is H, R^5= -CH_2SiCl_3, when R^6 is Me, R^3=-SiCl_3; R^4 is H, when R5=R6=-CH_2SiCl_3, R^3=Et, SiMe_2Cl, -SiMeCl_2, -SiCl_3, and m is integer number of 0-9.COPYRIGHT KIPO 2015
[2σ + 2σ + 2π]-Cycloaddition of quadricyclane to partially methylated chlorosilylalkenes
Chapala, Pavel P.,Bermeshev, Maxim V.,Lakhtin, Valentin G.,Genaev, Alexander M.,Tavtorkin, Alexander N.,Finkelshtein, Eugene Sh.
, p. 344 - 345 (2015/10/19)
[2σ + 2σ + 2π]-Cycloaddition of quadricyclane to trissilylated ethenes Cl3 - nMenSiCH=CSiMenCl3 - n(SiMe3 - nCln) (n = 1, 2) at 95 °C affords 3,3,4-trissilylated exo-tricyclo[4.2.1.02,5]non-7-enes. Tetrakis(trichlorosilyl)ethene does not react with quadricyclane.
METHOD OF PREPARING HALOGENATED SILAHYDROCARBYLENES
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Paragraph 0038, (2014/05/07)
A method comprises separate and consecutive steps (i) and (ii). Step (i) includes contacting a copper catalyst with hydrogen gas and a halogenated silane monomer at a temperature of 500 °C to 1400 °C to form a silicon-containing copper catalyst comprising at least 0.1 % (w/w) of silicon. Step (ii) includes contacting the silicon-containing copper catalyst with an organohalide at a temperature of 100°C to 600 °C to form a reaction product. The organohalide has formula HaCbXc, where X is a halogen atom, subscript a is an integer of 0 or more, subscript b is an integer of 1 or more, and subscript c is an integer of 2 or more. The method produces a reaction product. The reaction product includes a halogenated silahydrocarbylene.
PRODUCTION METHOD FOR LINEAR AND CYCLIC TRISILAALKANE
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Page/Page column 5, (2011/04/19)
The present invention relates to a preparation method for a linear or cyclic trisilaalkane which is a substance useful in the preparation of polycarbosilane and silicon carbide precursors. Linear or cyclic trisilaalkane and organic trichlorosilane derivatives can be synthesized simultaneously and in high yield by reacting bis(chlorosily)methane having a Si—H bond, either alone or together with an organic chloride, using a quaternary organic phosphonium salt compound as a catalyst. Further, since the catalyst can be recovered after use, the present invention is very economical and is thus effective for mass-producing precursors for organic/inorganic hybrid substances.
Phosphine-Catalyzed Si-C Coupling of Bissilylmethanes: Preparation of Cyclic (Cl2SiCH2)2 and Linear Cl 2Si(CH2SiCl3)2 via Silylene and Silene Intermediates
Hong, Soon Hyun,Hyun, Sang Il,Jung, Il Nam,Han, Won-Sik,Kim, Min-Hye,Yun, Hoseop,Nam, Suk-Woo,Kang, Sang Ook
experimental part, p. 687 - 691 (2010/05/15)
Cyclic and linear carbosilanes, (Cl2SiCH2) 2 (2) and Cl2Si(CH2SiCl3) 2 (3), were produced from phosphine-catalized Si-C coupling reactions of bissilylmethanes, HCl2SiCH2SiX1X 2Cl (X1, X2 = Cl (1), X1 = H, X 2 = Cl (7), and X1 = Me, X2 = Cl (8)). The formation of compounds 2 and 3 suggested competing reaction pathways, involving dichlorosilene [CH2=SiCl2] and dichlorosilylene [:SiCl2] intermediates. Each intermediate was either proposed by the product isolation of the trimerized product (3) or confirmed by trapping experiments with 2,3-dimethylbutadiene and methylene chloride.
Si-C coupling reaction of polychloromethanes with HSiCl3 in the presence of Bu4PCl: Convenient synthetic method for bis(chlorosilyl)methanes
Jung, Dong Euy,Kang, Seung-Hyun,Han, Joon Soo,Lim, Weon Cheol,Park, Young-ae W.,Yoo, Bok Ryul
, p. 3901 - 3906 (2008/03/12)
Coupling reaction of polychloromethanes CH4-nCln (n = 2-4) with HSiCl3 in the presence of tetrabutylphosphonium chloride (Bu4PCl) as a catalyst occurred at temperatures ranging from 30 °C to 150 °C. The reactivity of polychloromethanes increases as the number of chlorine-substituents on the carbon increases. In the reactions of CCl4 with HSiCl3, a variety of coupling products such as bis(chlorosilyl)methanes CH2(SiCl3)(SiXCl2) [X = Cl (1a), H (1b)], (chlorosilyl)trichloromthanes Cl3CSiXCl2 [X = Cl (2a), H (2b)], and (chlorosilyl)dichloromthanes Cl2HCSiXCl2 [X = Cl (3a), H (3b)] were obtained along with reductive dechlorination products such as CHCl3 and CH2Cl2 depending on the reaction temperature. In the reaction of CCl4, 2a is formed at the initial stage of the coupling reaction and converted to give CHCl3 at low temperature of 30 °C, to give 1a, 3a, and CHCl3 at 60 °C, and to afford 1a as major product and CH2Cl2 in competition above 100 °C. Si-H bond containing silylmethanes can be formed by the H-Cl exchange reaction with HSiCl3. Reaction of CHCl3 with HSiCl3 took placed at 80 °C to give three compounds 1a, 3a, and CH2Cl2, and finally 3a was converted to give 1a and CH2Cl2 at longer reaction time. While the condition for the reaction of CH2Cl2 with HSiCl3 required a much higher temperature of 150 °C. Under the optimized conditions for synthesizing bis(chlorosilyl)methanes 1a,b, a mixture of 1a and 1b were obtained as major products in 65% (1a:1b = 64:1) and 47% (42:5) yields from the reaction of CCl4 and CHCl3 at 100 °C for 8 h, respectively, and in 41% (34:7) yield from that of CH2Cl2 at 170 °C for 12 h. In the Si-C coupling reaction of polychloromethanes with HSiCl3, it seems likely that a trichlorosilyl anion generated from the reaction of HSiCl3 with Bu4PCl is an important key intermediate.
Processes for manufacturing organochlorosilanes and dipodal silanes and silanes made thereby
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Page/Page column 7, (2010/02/10)
Processes are provided for producing organchlorosilanes and dipodal silanes in which an organic halide or alkene or chloralkene is reacted with a hydridochlorosilane in the presence of a quarternary phosphonium salt catalyst by providing sufficient heat to effect a dehydrohalogenative coupling reaction and/or a hydrosilylation reaction and venting the reaction to control reaction pressure and to remove gaseous byproducts from the reaction. The processes are preferably continuous using a catalyst in fluid form at reaction pressures not exceeding about 600 psi. The reactions may be carried out substantially isothermally and/or isobarically, for example in a plug flow reactor or continuous stirred tank reactor. The processes may produce novel silylated compounds including 1,2-bis(trichlorosilyl)decane or 1,2-bis(trimethoxysilyl)decane.
