- Synthesis and structure of novel Si-substituted silylpropyl derivatives of 2-mercaptobenzoxazole and 2-mercaptobenzothiazole
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[Figure not available: see fulltext.] A previously unknown carbofunctional (trimethoxysilyl)propyl derivative of the 2-mercaptobenzoxazole, C6H4NOCS(CH2)3Si(OMe)3, containing a tetracoordinated silicon atom was synthesized by nucleophilic substitution of the chlorine atom in the (3-chloropropyl)-trimethoxysilane with the benzoxazol-2-ylsulfanyl group. The reaction of 2-[(trimethoxysilyl)propylsulfanyl]benzoxazole or –benzothiazole with boron trifluoride etherate led to a previously unknown hydrolytically unstable Si-fluoropropyl derivatives of 2-mercaptobenzoxazole or 2-mercaptobenzothiazole, C6H4N(Y)CS(CH2)3SiF3 (Y = O, S). By transesterification of 2-[(trimethoxysilyl)-propylsulfanyl]benzoxazole by tris(2-hydroxyethyl)amine, a new silatranylpropyl derivative of 2-mercaptobenzoxazole containing an intramolecular coordination bond N→Si and a pentacoordinated silicon atom, C6H4NOCS(CH2)3Si(OCH2CH2)3N, was obtained.
- Grebneva, Ekaterina А.,Bolgova, Yuliya I.,Trofimova, Olga M.,Albanov, Aleksander I.,Borodina, Tatyana N.
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Read Online
- Synthetic process of silicon-based imidazole epoxy resin curing agent
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The invention discloses a synthetic process of a silicon-based imidazole epoxy resin curing agent and belongs to the technical field of synthesis of curing agents. The synthetic process comprises the following steps: taking chloropropyl trichlorosilane and alcohol as raw materials, synthesizing chloropropyl siloxane by adopting a continuous method and then conducting reaction with an imidazole substance to obtain the silicon-based imidazole epoxy resin curing agent. The synthetic process of the silicon-based imidazole epoxy resin curing agent, disclosed by the invention, has the benefits that some raw materials used in the production process are simple and easy to obtain; in the whole production process, conditions are milder, the operation is simple, the equipment requirements are low, and high temperature, high pressure and other special processes are not required, so that the safety and the economy are good; wastewater containing COD is not generated, and byproducts are less; in the first step of esterification, no waste is generated, by-product hydrochloric acid is also a product with economic benefits, and the influence on the environment is less; chloropropyl silane is continuously produced, so that the reaction is favorably promoted, and the by-products are reduced.
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Paragraph 0018
(2017/07/21)
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- Synthesis and properties of functionalized alkylalkoxysilanes
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A method of chloroalkylalkoxysilanes synthesis scalable to pilot production has been proposed. Morpholinotrialkoxysilanes have been prepared and studied as vulcanizing agents for low-molecular silicone rubbers. The reaction of N-morpholinomethyltrialkoxysilanes with triethanolamine has afforded N-[(silatranyl)-methyl]morpholine; it has been studied by X-ray analysis.
- Lebedev,Minas’yan,Abramkin,Sheludyakov,Kuzmina,Lebedeva,Surikov,Rybakov
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p. 1859 - 1863
(2016/10/04)
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- Synthesis of a multifunctional alkoxysiloxane oligomer
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An alkoxysiloxane oligomer (1, SiMe[OSi(CHCH2)(OMe)2][OSi(CH2)3Cl(OMe)2]2), containing vinyl and chloropropyl groups, was synthesized as a precursor for sol-gel synthesis. Di-tert-butoxymethylhydroxysilane (t-BuO)2MeSiOH was reacted with (MeO)2(CH2CH)SiCl to form (t-BuO)2MeSiOSi(CHCH2)(OMe)2 which was further alkoxysilylated with Cl(CH2)3SiCl(OMe)2 to form 1. The 1H, 13C, 29Si NMR and HR-MS data confirmed the formation of 1, indicating the successful synthesis of an alkoxysiloxane oligomer possessing different kinds of functional groups by a chemoselective route. Hydrolysis of 1 under acidic conditions was completed in a few hours. The solution state 29Si NMR spectra of samples hydrolyzed and condensed at various reaction times show no signals due to species generated by the cleavage of the siloxane bonds in 1, indicating the validity of the synthesized substance as a precursor for the formation of hybrids with homogeneously distributed functional groups. Intramolecular condensation of 1 to form cyclic trisiloxane units proceeds more preferentially than intermolecular condensation.
- Yoshikawa, Masashi,Wakabayashi, Ryutaro,Tamai, Misa,Kuroda, Kazuyuki
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supporting information
p. 5362 - 5368
(2014/12/11)
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- Hydrosilylation Synthesis of Haloalkylorganosilanes Using Peroxide Promoters
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This invention is directed to a process for producing a haloorganoalkoxysilane product comprising reacting an olefinic halide, an alkoxysilane, a catalytically effective amount of ruthenium-containing catalyst; and a reaction-promoting effective amount of a peroxy compound, optionally in the presence of an electron-deficient aromatic compound.
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Paragraph 0116-0120
(2014/05/07)
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- METHOD OF PRODUCING A HYDROLYZABLE SILICON-CONTAINING COMPOUND
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The present invention provides a safe, inexpensive, and high yield means of producing a hydrolyzable silicon-containing compound, e.g., an organooxysilane and the like. A compound (A) represented by the general formula R1-O-R2 wherein R1 represents a C4-30, substituted or unsubstituted, tertiary alkyl group or aralkyl group and R2 represents a C1-30, substituted or unsubstituted, monovalent hydrocarbyl group or acyl group, is reacted in the presence of a Lewis acid catalyst with a halosilane (B) represented by the general formula R3mSiX4-m wherein R3 represents the hydrogen atom or a C1-30 substituted or unsubstituted monovalent hydrocarbyl group, X is independently bromine or chlorine, and m represents an integer from 0 to 3.
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Page/Page column 18-19; 20
(2012/07/14)
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- Practical conversion of chlorosilanes into alkoxysilanes without generating HCl
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Alcohol-free: A versatile, efficient, and practical synthesis of alkoxysilanes without generation of HCl involves the reaction of chlorosilanes with unsymmetrical ethers in the presence of a Lewis acid (see scheme). The reaction proceeds through selective cleavage of C-O bonds and is superior to conventional processes. Industrially feasible reagents are used and only one by-product results. Copyright
- Wakabayashi, Ryutaro,Sugiura, Yasushi,Shibue, Toshimichi,Kuroda, Kazuyuki
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supporting information; experimental part
p. 10708 - 10711
(2011/12/05)
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- PROCESS FOR THE PREPARATION OF HALOALKYLALKOXYSILANCS AND HALOALKYLHALOSILANES
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This invention involves a process for the preparation of haloalkylalkoxysilanes and haloalkylhalosilancs. The process comprises reacting an alkoxyhydridosilane or a halohydridosilanc silane with an alkenylhalide compound in the presence of a catalytic amount of an iridium containing catalyst. When a halohydridosilane is the silane rcactant. the resulting haloalkylhalosilane may be alkoxylatcd by reaction with a C1-C6, alcohol, In another aspect of the invention, the reacting is conducted under a reduced oκygen atmosphere to improve the catalyst activity and the yield of the resulting haloalkylhalosilane or halυalkylalkυx vsi lane.
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Page/Page column 22
(2009/10/22)
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- PROCESS FOR MAKING HALOORGANOALKOXYSILANES
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A haloorganoalkoxysilane is prepared by reacting an olefinic halide with an alkoxysilane in which the alkoxy group(s) contain at least two carbon atoms in a reaction medium to which has been added a catalytically effective amount of ruthenium-containing catalyst and a reaction-promoting effective amount of an electron-donating aromatic compound promoter. The process can be used to prepare, inter alia, chloropropyltriethoxysilane, which is a key intermediate in the manufacture of silane coupling agents.
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Page/Page column 11-12; 18
(2008/06/13)
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- Process for making haloorganoalkoxysilanes
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A haloorganoalkoxysilane is prepared by reacting an olefinic halide with an alkoxysilane in which the alkoxy group(s) contain at least two carbon atoms in a reaction medium to which has been added a catalytically effective amount of ruthenium-containing catalyst and a reaction-promoting effective amount of an electron-donating aromatic compound promoter. The process can be used to prepare, inter alia, chloropropyltriethoxysilane, which is a key intermediate in the manufacture of silane coupling agents.
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- Process for preparing low-chloride or chloride-free alkoxysilanes
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A process for preparing an alkoxysilane with an acidic chloride content of less than 10 ppm by weight, comprising: reacting a chlorosilane with an alcohol in a water-free and solvent-free phase to form a product mixture containing alkoxysilane and residual acidic chloride, with removal of resultant hydrogen chloride from the product mixture, then adding liquid or gaseous ammonia, in an amount corresponding to a stoichiometric excess, based on the content of acidic chloride, to form an ammonia-containing product mixture, treating the ammonia-containing product mixture at a temperature between 10 and 50 DEG C., wherein the ammonia and acidic chloride undergo neutralization, to form a crude product, and optionally, then separating off a salt formed in the course of neutralization, from the crude product, and recovering the alkoxysilane by distilling the crude product.
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- Process for removing acidic impurities from alkoxysilanes
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A process for removing acidic impurities from alkoxysilanes obtained from halogenosilanes and alcohols which inevitable contain small amounts of acidic impurities is described. In the process, at least one member selected from alkali metal salts of alcohols and amines having a great steric hindrance as having a bulky substituent is added to the alkoxysilane for a time sufficient to neutralize the acidic impurities and the mixture is purified by distillation to obtain a substantially acidic impurity-free alkoxysilane.
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- Packing for use in resolution
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The packing for use in resolution proposed for the liquid chromatography for particularly the opti-cal resolution of racemic compounds is prepared by reacting a silica gel carrier with a so-called silane treating agent to introduce a spacer part therein and chemically bonding it with a copper salt of a carboxylic or thiocarboxylic acid selected from the group consisting of optically active D- and L-2--acetizinecaroxylic acid, proline, hydroxyproline and allohydroxyproline. The steric bulkiness, the distance between the silica gel and the optically active group and the degree of hydrophobicity are specified so as to obtain an excellent resolving power.
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- Novel process for the preparation of halopropyltrialkoxysilanes and halopropylalkylalkoxysilanes
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A process for the preparation of halopropyltrialkoxysilanes and halopropylalkylalkoxysilanes comprising the hydrosilation of allyl halides (including substituted allyl halides) with trialkoxysilanes and alkylalkoxy silanes over specific iridium-containing catalysts.
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- Process for the preparation of organoalkoxysilanes
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An improvement in a process for the esterification of a organochlorosilane by feeding alcohol into a chlorosilane maintained within a reaction zone without said alcohol contacting said chlorosilane in the gas phase wherein the esterification is performed stepwise with extraction of hydrogen chloride which has developed, the improvement which comprises employing in at least a final esterification step an organochlorosilane of the formula wherein R represents an optionally halogen-substituted alkyl radical which can also contain an oxygen or sulfur atom in the chain, or a halogen or a NO2 group or a protected phenolic group containing aryl radical, a equals 0, 1, or 2, b equals 1 or 2, and a+b amounts to a maximum of 3, said final esterification step being performed with the addition of heat.
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