trichloro(phenyl)silane

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Triethylamine (3.9 g) was added to a flask containing 83.3 g of the crude product mixture described in Example 1. This mixture was stripped by the process described in Example 1. The volatiles were condensed and analyzed by GC-TCD. About 77.4 g of a liquid was recovered comprising 24.7 g of diphenyldichlorosilane (yield of 77 percent), 1.4 g of phenyldichlorosilane, 24.5 g of phenyltrichlorosilane, and 10.1 g of benzene. condensed About 77.4 g of a liquid was recovered

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Eaborn et al., J. Organometal. Chem. 4:489 (1965), describes a process where phenyltrimethylsilane and trichlorosilane are reacted at 500° C. in the gas phase to give phenyltrichlorosilane and trimethylsilane. are reacted at 500° C. in the gas phase

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Eaborn et al., J. Organometal. Chem. 4:489 (1965). describes a process where phenyltrimethylsilane and trichlorosilane are reacted at 500° C. in the gas phase to give phenyltrichlorosilane and trimethylsilane. are reacted at 500° C. in the gas phase

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Eaborn et al., J. Organometal. Chem. 4:489 (1965). describes a process where phenyltrimethylsilane and trichlorosilane are reacted at 500° C. in the gas phase to give phenyltrichlorosilane and trimethylsilane. are reacted at 500° C. in the gas phase

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Anhydrous tetrahydrofuran (125 mL) was put into a reactor with magnesium (5.7 g, 0.24 mol) and molecular sieves 4A which had been dehydrated and deaerated, followed by charging of argon gas. A small amount of iodine was slowly added to the mixture. (S)-(+)-1-bromo-2-methylbutane (30 g, 0.20 mol) was added dropwise to the slowly stirred mixture so that the reaction mixture was gradually refluxed. After the reaction was complete, the obtained Grignard reagent was transferred to a dropping funnel. The Grignard reagent was added dropwise to a solution being stirred containing phenyltrichlorosilane (50 g, 0.24 mol) in anhydrous tetrahydrofuran (50 mL) in another reactor which had been dehydrated and deaerated, followed by charging of argon gas, at 40° C.-50° C. The reaction mixture was then stirred overnight at room temperature. Hexane (500 mL) was added to the reaction mixture, and the resulting mixture was filtered under pressure, followed by fractional distillation of the filtrate to provide the desired product. was gradually refluxed by charging of argon gas, at 40° C.-50° C The reaction mixture was then stirred overnight at room temperature the resulting mixture was filtered under pressure followed by fractional distillation of the filtrate

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Anhydrous tetrahydrofuran (125 mL) was put into a reactor with magnesium (5.7 g, 0.24 mol) and molecular sieves 4A which had been dehydrated and deaerated, followed by charging of argon gas. A small amount of iodine was slowly added to the mixture. (S)-(+)-1-bromo-2-methylbutane (30 g, 0.20 mol) was added dropwise to the slowly stirred mixture so that the reaction mixture was gradually refluxed. After the reaction was complete, the obtained Grignard reagent was transferred to a dropping funnel. The Grignard reagent was added dropwise to a solution being stirred containing phenyltrichlorosilane (50 g, 0.24 mol) in anhydrous tetrahydrofuran (50 mL) in another reactor which had been dehydrated and deaerated, followed by charging of argon gas, at 40° C.-50° C. The reaction mixture was then stirred overnight at room temperature. Hexane (500 mL) was added to the reaction mixture, and the resulting mixture was filtered under pressure, followed by fractional distillation of the filtrate to provide the desired product. was gradually refluxed by charging of argon gas, at 40° C.-50° C The reaction mixture was then stirred overnight at room temperature the resulting mixture was filtered under pressure followed by fractional distillation of the filtrate

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a round flask (internal volume: 1000 ml) equipped with a three-way stopcock, 40 g of granular magnesium (particle size: 20 to 1000 μm) and 20 g of lithium chloride as a catalyst were fed, and the internal of the reaction vessel (flask) was dried with heating at 50° C. under a reduced pressure of 1 mmHg (=133 kPa). Thereafter, dry argon gas was introduced into the reaction vessel, 500 ml of tetrahydrofuran (THF) pre-dried with sodium-benzophenone ketyl was added thereto, and the mixture was stirred at 25° C. for about 60 minutes. To the reaction mixture were added 31.7 g (0.15 mol) of phenyltrichlorosilane purified by distillation and 34.5 g (0.3 mol) of methyldichlorosilane purified by distillation by the use of a syringe, and the resulting mixture was stirred at 25° C. for about 24 hours. After completion of the reaction, 1000 ml of 1N (=1 mol/L) hydrochloric acid was put in the reaction mixture, and the reaction mixture was subjected to extraction with 500 ml of toluene. The washing of the toluene layer with 200 ml aliquots of purified water was repeated ten times, and the toluene layer was dried with anhydrous magnesium sulfate, and then toluene was distilled off to give a phenyltrichlorosilane-methyldichlorosilane copolymer (the former/the latter (molar ratio)=1/2) (weight-average molecular weight: 3500). the internal of the reaction vessel (flask) was dried Thereafter, dry argon gas was introduced into the reaction vessel, 500 ml of tetrahydrofuran (THF) pre-dried with sodium-benzophenone ketyl was added purified by distillation by the use of a syringe the resulting mixture was stirred at 25° C. for about 24 hours After completion of the reaction, 1000 ml of 1N (=1 mol/L) hydrochloric acid the reaction mixture was subjected to extraction with 500 ml of toluene The washing of the toluene layer with 200 ml aliquots of purified water the toluene layer was dried with anhydrous magnesium sulfate toluene was distilled off

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a round flask (internal volume: 1000 ml) equipped with a three-way stopcock, 25 g of granular magnesium (particle size: 20 to 1000 μm) and 20 g of lithium chloride as a catalyst were fed, and the internal of the reaction vessel (flask) was dried with heating at 50° C. under a reduced pressure of 1 mmHg (=133 kPa). Thereafter, dry argon gas was introduced into the reaction vessel, 500 ml of tetrahydrofuran (THF) pre-dried with sodium-benzophenone ketyl was added thereto, and the mixture was stirred at 25° C. for about 60 minutes. To the reaction mixture were added 63.5 g (0.3 mol) of phenyltrichlorosilane purified by distillation and 34.5 g (0.3 mol) of methyldichlorosilane purified by distillation by the use of a syringe, and the resulting mixture was stirred at 25° C. for about 24 hours. After completion of the reaction, 1000 ml of 1N (=1 mol/L) hydrochloric acid was put in the reaction mixture, and the reaction mixture was subjected to extraction with 500 ml of toluene. The washing of the toluene layer with 200 ml aliquots of purified water was repeated ten times, and the toluene layer was dried with anhydrous magnesium sulfate, and then toluene was distilled off to give a phenyltrichlorosilane-methyldichlorosilane copolymer (the former/the latter (molar ratio)=1/1) (weight-average molecular weight: 2500). the internal of the reaction vessel (flask) was dried Thereafter, dry argon gas was introduced into the reaction vessel, 500 ml of tetrahydrofuran (THF) pre-dried with sodium-benzophenone ketyl was added purified by distillation by the use of a syringe the resulting mixture was stirred at 25° C. for about 24 hours After completion of the reaction, 1000 ml of 1N (=1 mol/L) hydrochloric acid the reaction mixture was subjected to extraction with 500 ml of toluene The washing of the toluene layer with 200 ml aliquots of purified water the toluene layer was dried with anhydrous magnesium sulfate toluene was distilled off