tetramethyl silicate

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: The fine particles used were composite inorganic fine particles of silica and titania (average particle diameter: 100 nm). The fine particles were produced in the following manner according to the method disclosed in Production Example and Example of JP-A-7-2520. 140 g of methanol, 260 g of isopropanol and 100 g of aqueous ammonia (25% by weight) were charged in a 4-L glass reactor equipped with stirring blades to prepare a reaction solution, which was stirred while the temperature of the reaction solution was maintained to 40° C. 542 g of silicon tetramethoxide (Si(OMe)4, Methyl Silicate 39, a trade name, produced by Colcoat Co., Ltd.) was charged in a 3-L conical flask, and 195 g of methanol and 28 g of a 0.1% by weight aqueous solution of hydrochloric acid (obtained by diluting 35% hydrochloric acid, produced by Wako Pure Chemical Industries, Ltd. with water to 1/1,000) were added thereto under stirring, followed by further stirring for about 10 minutes. Subsequently, a solution obtained by diluting 300 g of titanium tetraisopropoxide (Ti(O-i-Pr)4, A-1 (TPT), a trade name, produced by Nippon Soda Co., Ltd.) with 634 g of isopropanol was added thereto to obtain a transparent uniform solution (copolycondensate of silicon tetraalkoxide and titanium tetraalkoxide). 1,699 g of the uniform solution and 480 g of aqueous ammonia (25% by weight) were simultaneously added dropwise to the aforementioned reaction solution over 2 hours at a small dropping rate in the initial stage, which was gradually increased toward the final stage. After completing the dropwise addition, the resulting cohydrolyzate was filtered and dried at 50° C. to remove the organic solvents, and it was then dispersed in water to obtain fine particles having a concentration of 10% by weight and a refractive index of 1.56. The fine particles were produced in the following manner equipped with stirring blades to prepare a reaction solution, which

Conditions: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: The fine particles used were composite inorganic fine particles of silica and titania (average particle diameter: 100 nm). The fine particles were produced in the following manner according to the method disclosed in Production Example and Example of JP-A-7-2520. 140 g of methanol, 260 g of isopropanol and 100 g of aqueous ammonia (25% by weight) were charged in a 4-L glass reactor equipped with stirring blades to prepare a reaction solution, which was stirred while the temperature of the reaction solution was maintained to 40° C. 542 g of silicon tetramethoxide (Si(OMe)4, Methyl Silicate 39, a trade name, produced by Colcoat Co., Ltd.) was charged in a 3-L conical flask, and 195 g of methanol and 28 g of a 0.1% by weight aqueous solution of hydrochloric acid (obtained by diluting 35% hydrochloric acid, produced by Wako Pure Chemical Industries, Ltd. with water to 1/1,000) were added thereto under stirring, followed by further stirring for about 10 minutes. Subsequently, a solution obtained by diluting 300 g of titanium tetraisopropoxide (Ti(O-i-Pr)4, A-1 (TPT), a trade name, produced by Nippon Soda Co., Ltd.) with 634 g of isopropanol was added thereto to obtain a transparent uniform solution (copolycondensate of silicon tetraalkoxide and titanium tetraalkoxide). 1,699 g of the uniform solution and 480 g of aqueous ammonia (25% by weight) were simultaneously added dropwise to the aforementioned reaction solution over 2 hours at a small dropping rate in the initial stage, which was gradually increased toward the final stage. After completing the dropwise addition, the resulting cohydrolyzate was filtered and dried at 50° C. to remove the organic solvents, and it was then dispersed in water to obtain fine particles having a concentration of 10% by weight and a refractive index of 1.56. The fine particles were produced in the following manner equipped with stirring blades to prepare a reaction solution, which

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Under an inert gas, 24.2 g magnesium chips (1.0 mol) were combined with about 20 ml methyl-tert-butylether, an iodine crystal and 3.1 g 2-chloropropane (0.04 mol). To start the reaction a solution of 61.9 g tetramethoxysilane (0.41 mol) and 75.4 g 2-chloropropane (0.96 mol) in 140 ml methyl-tert-butylether was added dropwise, with stirring, to the first mixture at a rate to maintain a moderate reflux. After addition of the solution, the reaction was allowed to reflux for six more hours. After cooling the reaction mixture, 6.0 g methanol (0.19 mol) was added, the mixture was stirred for a few minutes and then the resulting precipitate was removed by filtration. After washing the filter cake with several portions of methyl-tert-butylether, the solvent was distilled from the combined filtrates. The remaining residue consisted of 70.5 g diisopropyldimethoxysilane (98% of the theoretical yield) which had a purity of 98% according to GC. Triisopropylmethoxysilane was not detected by GC. was added dropwise to maintain a moderate reflux After addition of the solution to reflux for six more hours was added the mixture was stirred for a few minutes the resulting precipitate was removed by filtration After washing the filter cake with several portions of methyl-tert-butylether the solvent was distilled from the combined filtrates theoretical yield) which

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Under an inert gas, 24.2 g magnesium chips (1.0 mol) were combined with about 20 ml methyl-tert-butylether, an iodine crystal and 3.1 g 2-chloropropane (0.04 mol). To start the reaction a solution of 61.9 g tetramethoxysilane (0.41 mol) and 75.4 g 2-chloropropane (0.96 mol) in 140 ml methyl-tert-butylether was added dropwise, with stirring, to the first mixture at a rate to maintain a moderate reflux. After addition of the solution, the reaction was allowed to reflux for six more hours. After cooling the reaction mixture, 6.0 g methanol (0.19 mol) was added, the mixture was stirred for a few minutes and then the resulting precipitate was removed by filtration. After washing the filter cake with several portions of methyl-tert-butylether, the solvent was distilled from the combined filtrates. The remaining residue consisted of 70.5 g diisopropyldimethoxysilane (98% of the theoretical yield) which had a purity of 98% according to GC. Triisopropylmethoxysilane was not detected by GC. was added dropwise to maintain a moderate reflux After addition of the solution to reflux for six more hours was added the mixture was stirred for a few minutes the resulting precipitate was removed by filtration After washing the filter cake with several portions of methyl-tert-butylether the solvent was distilled from the combined filtrates theoretical yield) which

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Example 2 was repeated except that 0.04 gram of rubidium formate was used as the alkali carboxylate catalyst component and reaction time was 4.0 hours. Under these conditions 5.2 grams of methyltrimethoxysilane; 44.0 grams of tetramethoxysilane were produced; and 14.0 grams of methanol was unreacted. Of the total organosilanes in the distillation product 10.5 percent was methyltrimethoxysilane.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A 3-neck 1 L flask was filled with magnesium turnings (5 g), THF (200 g) and tetramethoxysilane (50 g), and heated to reflux. 2-Bromothianthrene (40 g), prepared analogously to Example 3A was added to the flask in 10 g portions. Grignard started within 10 minutes. The reaction was allowed to cool for 1 hour, after which magnesium salts were precipitated with hexanes (200 mL). GC/MS of the solution showed that along with some thianthrene, 2-(trimethoxysilyl)thianthrene was obtained in ˜60% yield (FIG. 7). heated to reflux was added to the flask in 10 g portions to cool for 1 hour after which magnesium salts were precipitated with hexanes (200 mL)

Conditions: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 4.1 ml of the tetrahydrofuran solution of magnesium 2-(1,3-butadienyl)chloride and 6 ml of dried tetrahydrofuran were charged into a reactor in the stream of argon. Subsequently, the reactor was cooled down to 0° C., followed by gentle dropping of 1.2 ml (8 mmols) of tetramethoxysilane. While the reaction temperature was kept at 0° C., the reaction was continued for 30 minutes. After completion of the reaction, the solvent was distilled off to obtain 2-(trimethoxy)silyl-1,3-butadiene (yield: 65%). was kept at 0° C. After completion of the reaction the solvent was distilled off