Shin-etsu Chemical Co., Ltd.

Matsushita Electric Industrial Co., Ltd.

Matsushita Electrical Industrial Co., Ltd.

Mikio Endo

Tohru Kubota

Toshinobu Ishihara

Kazufumi Ogawa

Norihisa Mino

Katsuhiro Uehara

Akira Yamamoto

Minoru Takamizawa

Masaki Takeuchi

Yoichi Tonomura

Yasuhisa Tanaka

Toshio Shinohara

Yasufumi Kubota

Satoshi Uchida

Katsuya Takemura

Shigehiro Nagura

Kenji Funatsu

Ikuo Fukui

Kanji Murofushi

Hiroshi Umezawa

Kazuyuki Asakura

Katsuyuki Oikawa

Hitoyuki Araki

Toru Kubota

Takeo Koshimura

Yasuhiro Kawase

Takeo Arai

A bissilylnorbornane compound is prepared by reacting 2,5-norbornadiene with a hydrogenchlorosilane in the presence of a mixture of a palladium compound and a phosphite or a palladium complex having a phosphate ligand as a catalyst. The bissilylnorbornane compound can be produced in high yields while suppressing formation of by-product nortricyclene.

Preparation of bissilylnorbornane compounds

A halopropyldimethylchlorosilane is prepared by reacting dimethylchlorosilane with an allyl halide in the presence of an iridium catalyst. The reaction is effected in the presence of an internal olefin compound, typically 1,5-cyclooctadiene. The internal olefin compound suppresses deactivation of the iridium catalyst during reaction. Using a smaller amount of the iridium catalyst, the process produces the halopropyldimethylchlorosilane in high yields.

Preparation of halopropyldimethylchlorosilanes

A (meth)acryloxy-bearing alkoxysilane is isolated and purified to a high purity by distilling a reaction solution containing the (meth)acryloxy-bearing alkoxysilane in a thin-layer distillation device at a temperature of 90-160&deg; C. and a vacuum of 1-15 mmHg. The resulting alkoxysilane product does not give rise to the quality problem that the product will gradually whiten during storage owing to contact with air. The occurrence of self-polymerization of the alkoxysilane is restrained.

Distillation of (meth) acryloxy-bearing alkoxysilane

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.

Preparation of bis(3-aminopropyldimethylsilyl)benzene compounds

By reacting 4-vinyl-1-cyclohexene with a hydrogenchlorosilane compound in the presence of a platinum catalyst to give a reaction solution containing a monosilyl compound, removing the residual 4-vinyl-1-cyclohexene and isomers thereof from the reaction solution, and reacting the monosilyl compound again with the hydrogenchlorosilane compound, an organic silicon compound in which the two double bonds in 4-vinyl-1-cyclohexene have been hydrosilylated is produced in high yields.

Hydrosilylation of 4-vinyl-1-cyclohexene

A hydroxyl group-containing compound is silylated by reacting it with an organohydrosilane compound in the presence of a ruthenium complex catalyst having carbonyl groups as ligands. Silylation takes place in a short time while the amount of the catalyst is minimized.

Silylation of hydroxyl group-containing compound

By subjecting to hydrosilylation a hydrogendimethylalkoxysilane compound and an N-silylated allylamine compound in the presence of a platinum catalyst, adding an alcohol to the reaction product to effect desilylation reaction, and hydrolyzing the resulting 3-aminopropyldimethylalkoxysilane compound, 1,3-bis(3-aminopropyl)tetramethyldisiloxane is prepared. The end product free of isomers and of quality can be prepared through simple steps, at a low cost and in high yields.

Preparation of 1,3-bis(3-aminopropyl)tetramethyldisiloxane

Disclosed is a novel organosilicon-containing derivative of pullulan of which an organopolysiloxane moiety having a silethylene linkage is bonded to the glucose residue of pullulan through a urethane linkage. Different from conventional organopolysiloxane-modified pullulans, the inventive derivative is stable against attack of water and exhibits unique properties as a combination of the properties inherent in pullulan and in silicones. The organosilicon-containing pullulan of the invention can be easily prepared under mild reaction conditions by reacting an isocyanato group-containing organopolysiloxane with the glucosic hydroxy groups of pullulan.

Siloxane-containing pullulan and method for the preparation thereof

By reacting a chloromonosilane or chlorodisilane with a halogenated hydrocarbon in a liquid phase in the presence of metallic aluminum or an aluminum alloy, a hydrocarbon group is substituted for at least one chlorine atom of the chlorosilane for introducing hydrocarbon into the chlorosilane. Silanes having a high degree of hydrocarbon substitution can be easily synthesized from chlorosilanes under moderate conditions and with high volumetric efficiency. The reagents used are aluminum or aluminum alloys and halogenated hydrocarbons which are inexpensive and readily available.

Method for introducing hydrocarbons into chlorosilanes

Disclosed are a conductive thienyl derivative monomolecular film covalently bonded to a substrate surface and method of manufacturing the same, and a silicon compound comprising 3-thienyl groups (thiophene derivative) used for forming the conductive monomolecular film and a method of manufacturing the same. A monomolecular ultrathin film comprising 3-thienyl groups and silicon groups is formed in the invention. The silicon compound used for forming the film is provided by reacting .omega.-(3-thienyl)-1-alkene compound to a monosilane derivative compound, in which three out of four hydrogen atoms of monosilane are replaced with halogen or alkoxy groups, in the presence of a transition metal catalyst. A substrate is dipped and held in a nonaqueous solution of the above-noted compound, thus chemically bonding the monomolecular film to the substrate surface. Furthermore, a thienyl derivative ultrathin film is formed by the electrolytic or catalytic polymerization of the monomolecular film.

Chemically adsorbed ultrathin film and its material, and method of

Disclosed are a conductive pyrrole derivative monomolecular film covalently bonded to a substrate surface and method of manufacturing the same, and a monomer used for forming the conductive pyrrole derivative monomolecular film and method of manufacturing the same. The invention relates to a monomolecular ultrathin film comprising 1-pyrrolyl groups and silicon groups. The monomer used for forming the film is provided by reacting .omega.-(1-pyrrolyl)-1-alkene compound to a monosilane derivative compound, in which three out of four hydrogen atoms of monosilane are replaced with halogen or alkoxy groups, in the presence of a transition metal catalyst. A substrate is dipped and held in a nonaqueous solution of the above-noted monomer, thus chemically bonding a monomolecular film to a substrate surface. Furthermore, a polypyrrole derivative ultrathin film is formed by the electrolytic or catalytic polymerization of the monomolecular film.

1-pyrrolyl silicon compounds, chemically adsorbed ultrathin film formed

The invention produces a 3-[N-(2-aminoethyl)]aminopropylalkoxysilane in high yields by reacting a 3-chloropropylalkoxysilane with ethylene diamine. A distillation pot is charged with ethylene diamine and heated above the boiling point of ethylene diamine for evaporating ethylene diamine, which is then condensed into a liquid. The liquid ethylene diamine is mixed for reaction with a 3-chloropropylalkoxysilane in such a proportion to give a molar ratio of ethylene diamine/3-chloropropylalkoxysilane of at least 12/1, thereby forming a 3-[N-(2-aminoethyl)]aminopropylalkoxysilane. The reaction solution is fed back to the pot where the unreacted ethylene diamine in the reaction solution is evaporated again and then condensed for use in a next cycle of reaction. The apparatus includes a distillation pot, a reflux condenser, a feed means and a reactor connected to form a recirculating system.

Method and apparatus for preparing

Dimethylchlorosilane and a triorganochlorosilane of the formula: R.sup.1 R.sup.2 R.sup.3 SiCl wherein R.sup.1, R.sup.2, and R.sup.3 are independently selected from monovalent hydrocarbon groups are concurrently prepared by reacting dimethyldichlorosilane with a SiH bond-containing silane compound of the formula: R.sup.1 R.sup.2 R.sup.3 SiH in the presence of a Lewis acid catalyst. The method is especially effective for concomitant preparation of dimethylchlorosilane and trimethylchlorosilane or t-butyldimethylchlorosilane in an inexpensive, simple, safe manner and in high yields.

Concurrent preparation of dimethylchlorosilane and triorganochlorosilane

A recording and reproducing device is provided. The device comprises a recording medium, a head giving and receiving recording signals to or from the recording medium, and a mechanism section and a circuit section giving and receiving the recording signals, wherein at least one protective film, and at least one fluorine-containing monomolecular film are formed in this order on the recording layer of the recording medium or on the surface of the head which comes into contact with said recording layer, wherein said protective film is a metal film, oxidized metal film, semi-conductor film, oxidized semi-conductor film, or organic monomolecular film, and wherein said fluorine-containing monomolecular film is formed by the chemical adsorption of a specific-type of silane compound that contains a perfluoroalkyl group at the molecular end on the surface of the protective film.

Recording and reproducing device which includes a protective film and a

A triorganomonohalogenosilane is prepared by reacting a triorganomonohydrosilane represented by the following general formula (I):

Growing community of inventors

Joetsu, Japan

Mikio Endo