- Preparation method of BDSB (1,4-bis(dimethyls-ilyl)benzene)
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The invention relates to a preparation method of BDSB (1,4-bis(dimethyls-ilyl)benzene) and relates to the technical field of chemical synthesis. Metallic sodium, TDA-1 (tris(3,6-dioxaheptyl)amine) andxylene are mixed and stirred at the temperature of 100-110 DEG C until the metallic sodium is changed into sodium sand, then, a mixture comprising p-dichlorobenzene, chlorodimethylsilane and xylene is dropwise added, the obtained mixture reacts at 100-110 DEG C, cooling is performed after the reaction ends, water is dropped, the obtain mixture is stirred and left to stand, an upper organic phaseis taken and subjected to reduced pressure rectification, and the BDSB is obtained. The yield and purity are high, the process is simpler, and the method is low in cost, easy to operate during production and suitable for industrial production.
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Paragraph 0012-0021
(2018/03/06)
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- POLYMER WITH ALTERNATING PHENYLENE SILICON AND SILOXANE STRUCTURE AND METHOD OF PRODUCING PRECURSOR OF THE SAME
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A polymer with alternating phenylene silicon and siloxane structure and a method of producing a precursor of the same are introduced to develop an autonomous synthesis process for para-phenylene disilanol monomer compounds and design a technique of purifying the polymer with alternating phenylene silicon and siloxane structure easily, so as to enable mass production of the polymer with alternating phenylene silicon and siloxane structure.
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Paragraph 0041
(2018/08/03)
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- With the turn of the silicon extension phenyl and elongated structure of polymer and its precursor for the preparation method (by machine translation)
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The present invention provides a silicon extension with the turn of phenyl and elongated structure of polymer and its precursor for the preparation method. In this way, development of para-bis-[...] silicon alkanol monomer compound of synthesized process, and further design with the turn of the silicon extension phenyl and elongated framework purification procedure is simple method for manufacturing the same, in order to provide with the turn of the silicon extension phenyl and elongated structure can be in the production of the polymer industry use. (by machine translation)
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Paragraph 0034
(2018/03/31)
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- Synthesis of heteroatomic bridged paracyclophanes
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Heteroatomic bridged paracyclophanes were obtained by two independent synthetic approaches. The required precursors consist of para R2SiCl (R = Me, iPr) substituted aromatic rings (2 and 4). They were subsequently functionalised by using NH3, [LiPH2(dme)] or LiAl(PH2)4. In the case of the Me-substituted species 2, the reaction with NH3 directly yielded the Si2N bridged paracyclophane 5. The Si2P incorporated derivative 10 was obtained by lithiation of p-C6H4(SiiPr2PH2)2 (9) and subsequent salt metathesis with the chlorosilane 4. The second approach involves the use of GaEt3 in the formation of four membered (GaPn)2 cycles (Pn = N, P). p-[C6H4{SiiPr2N(H)GaEt2}2]2 (11) and p-[C6H4{SiiPr2P(H)GaEt2}2]2 (12) represent the first examples of stable (GaPn)2cis isomers as the trans species did not appear in solution. Although 11 and 12 show a similar coordination pattern, they differ in the orientation of the aromatic systems: in the solid structure, 11 adopts a-for paracyclophanes so far unique-T-shape conformation of the phenyl rings, while 12 shows the predominant coplanar orientation. All cyclophanes were characterized by X-ray diffraction, elemental analysis, NMR and IR spectroscopy.
- Reuter,Maas,Reuter,Kilgenstein,Asfaha,Von H?nisch
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p. 4530 - 4541
(2017/04/10)
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- Silole-containing poly(silylenevinylene)s: Synthesis, characterization, aggregation-enhanced emission, and explosive detection
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Hydrosilylation polymerizations of 1,1-dimethyl-2,5-bis(4-ethynylphenyl)-3, 4-diphenylsilole with aromatic silylhydrides including 1,4-bis(dimethylsilyl) benzene, 4,4'-bis(dimethylsilyl)biphenyl, 2,5-bis(dimethylsilyl)thiophene, and 2,7-bis(dimethylsilyl)-9,9-dihexylfluorene in the presence of Rh(PPh 3)3Cl catalyst in refluxed tetrahydrofuran afford a series of silole-containing poly(silylenevinylene)s. Under optimum condition, the alkyne polyhydrosilylation reactions progress efficiently and regioselectively, yielding polymers with high molecular weights (Mw up to 95,300) and good stereoregularity (E content close to 99%) in high yields (up to 92%). The polymers are processable and thermally stable, with high decomposition temperatures in the range of 420-449 °C corresponding to 5% weight loss. They are weakly fluorescent in the solution state but become emissive in the aggregate and film states, demonstrating their aggregation-enhanced emission characteristics. The explosive sensing capabilities of the polymers are examined in both solution and aggregate states. The emissions of the polymers aggregates in aqueous mixture are quenched more efficiently by picric acid in an exponential pattern with high quenching constants (up to 27,949 L mol -1), suggesting that the polymers aggregates are sensitive chemosensors for explosive detection. 2012 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2012 A series of silole-containing poly(silylenevinylene)s are synthesized regioselectively in high yields. These polymers show aggregation-enhanced emission and sensitive response to explosives in aqueous media. Copyright
- Zhao, Zujin,Jiang, Tao,Guo, Yanju,Ding, Liyuan,He, Bairong,Chang, Zhengfeng,Lam, Jacky W. Y.,Liu, Jianzhao,Chan, Carrie Y. K.,Lu, Ping,Xu, Liwen,Qiu, Huayu,Tang, Ben Zhong
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experimental part
p. 2265 - 2274
(2012/07/14)
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- PREPARATION OF ORGANOSILICON INTERMEDIATE AND THEIR DERIVATIVES IN A NOVEL GRIGNARD PROCESS
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A one-step process for the preparation of organosilicon intermediates. The organosilicon intermediates comprise a group which includes such intermediates as 1,4-bis(dimethylsilyl)benzene, 1,4-bis(dimethylchlorosilyl)benzene, and their derivatives. The process comprises: combining a dihalobenzene with magnesium metal in a co-solvent mixture of an ether and an organic solvent and reacting them with an organosilicon compound of the general formula, R2bHcSiXd. The resulting mixture is allowed to react to completion. The resulting mixture is passed through a filtration device. The liquid, now free of solid magnesium halide, is subjected to a separation technique to recover the subject organosilicon intermediates and their derivatives.
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- Preparation of bis(3-aminopropyldimethylsilyl)benzene compounds
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1,2-, 1,3- or 1,4-bis(3-aminopropyldimethylsilyl)benzene is prepared by effecting hydrosilylation reaction between N,N-bis(trimethylsilyl)allylamine and 1,2-, 1,3- or 1,4-bis(dimethylsilyl)benzene in the presence of a platinum catalyst, followed by detrimethylsilylation reaction. The process is simple and inexpensive to synthesize the end compound in high yields without forming isomers.
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- Phenyldimethylsilyl-substituted ketenes and bisketenes
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The phenyldimethylsilyl-substituted monoketene PhMe2SiCH=C=O (1) and bisketene (PhMe2-SiC=C=O)2 (3) have been prepared and compared to the corresponding Me3Si- and t-BuMe2Si-substituted species. The 13C, 17O, and 29Si NMR spectra fit the pattern shown by other silylketenes and provide no evidence for transmission of a substituent effect of the Ph group through the silicon to the ketenyl group, as has been proposed for PhMe2Si-substituted radicals. The UV spectrum of 1 does show a longer λ and greater ∈ than for t-BuMe2SiCH=C=O, and this may indicate some interaction of the phenyl group with the ketene chromophore, while the greater reactivity of 1 in hydration compared to t-BuMe2SiCH=C=O is ascribed to the inductive effect of the phenyl. The very similar ring-opening reactivity of the bis(phenyldimethylsilyl)cyclobutenedione (6) to form 3 compared to the bis(Me3Si) analogues also provides no evidence of a significant interaction of the phenyl with the ketene. A new type of stabilized 1,8-bisketene based on the arylbis(dimethylsilyl) grouping, namely, 1,4-bis(ketenyldimethylsilyl)benzene (12), has been prepared for the first time.
- Liu, Ronghau,Marra, Romeo M.,Tidwell, Thomas T.
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p. 6227 - 6232
(2007/10/03)
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- Polycylopentadienyls: synthesis of arylsilylcyclopentadienyl compounds and their η5-complexes with tungsten
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A general route to arylsilylcyclopentadienyl compounds starting from 1,4-C6H4Br2, 2,6-C5NH3Br2 and 1,3,5-C6H3Br3 is described.The aryl bromides were treated with Mg/ClSiMe2H to give the aryldimethylsilanes 1,4-C6H4(SiMe2H)2, 2,6-C5NH3(SiMe2H)2, and 1,3,5-C6H3(SiMe2H)3 which after reaction with Cl2 or Br2 yielded the aryldimethylsilyl halides 1,4-C6H4(SiMe2Br)2, 2,6-C5NH3(SiMe2Br)2, 1,3,5-C6H3(SiMe2X)3 (X=Br or Cl) in excellent yields.The halide can be replaced by various cyclopentadienides to give aryldimethylsilylcyclopentadienes of the general type 1,4-C6H4(SiMe2Cp)2 and 1,3,5-C6H3(SiMe2Cp)3 (Cp=C5H5 (8,11), C5H3(t-C4H9)2 (9, 12), C5HMe4 (10, 13)).Compounds C6H5(SiMe2(C5H5)), 1,4-C6H4(SiMe2(C5H5))2 (8) and 1,3,5-C6H3(SiMe2(C5H5))3 (11) were in turn treated with NaH, (MeCN)3W(CO)3, and MeI to give the η5-bound complexes C6H5(SiMe2(C5H4)W(CO)3Me) (14), 1,4-C6H4(SiMe2(C5H4)W(CO)3Me)2 (15), 1,3,5-C6H3(SiMe2(C5H4)W(CO)3Me)3 (16), which contain up to three half-sandwich units within one molecule.
- Plenio, Herbert
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