trichloro(hexyl)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:

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: The present experiement was described as shown in the following typical experimental No. 63 in Table 13. The reaction was carried out under the same condition as in Example 3, except that the same amount of t-butyl chloride was, used as the hydrogen chloride source. A mixture of 2-chloropropane and t-butyl chloride having the mixing ratio of 1:6 was reacted with metallic silicon at 280° C. to give 16.1 g of reaction products. The reaction products contained 5.9 g (45.2%) of 1,1-dichloro-1-silaheptane and 1.4 g (9.0%) of 1,1,1-trichloro-1-silaheptane. As other by-products, 31.1 g (13.2%) of 1-chlorohexane which is remained unreacted, 1.1 g (17.9%) of hexene, 2.5 g of trichlorosilane, and unconfirmed materials were obtained. was reacted with metallic silicon at 280° C. to give 16.1 g of reaction products

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

実験手順: The present experiement was described as shown in the following typical experimental No. 63 in Table 13. The reaction was carried out under the same condition as in Example 3, except that the same amount of t-butyl chloride was, used as the hydrogen chloride source. A mixture of 2-chloropropane and t-butyl chloride having the mixing ratio of 1:6 was reacted with metallic silicon at 280° C. to give 16.1 g of reaction products. The reaction products contained 5.9 g (45.2%) of 1,1-dichloro-1-silaheptane and 1.4 g (9.0%) of 1,1,1-trichloro-1-silaheptane. As other by-products, 31.1 g (13.2%) of 1-chlorohexane which is remained unreacted, 1.1 g (17.9%) of hexene, 2.5 g of trichlorosilane, and unconfirmed materials were obtained. was reacted with metallic silicon at 280° C. to give 16.1 g of reaction products

反応条件: temp:150.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a 25 ml oven dried stainless steel tube, 0.15 g (0.75 mmol) of tri-n-butylphosphine, 0.90 g (7.5 mmol) of 1-chlorohexane, and 5.08 g (37.5 mmol) of trichlorosilane were added under a dry nitrogen atmosphere. After sealing the cylinder with a valve, the reactor was maintained at 150° C. for 12 hrs. The resulting mixture was distilled to yield 1.1 g of n-hexyltrichlorosilane (bp; 215-219° C., yield; 65%). The resulting mixture was distilled

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

実験手順: Anhydrous diethyl ether (100 mL) was put into a reactor with magnesium (5.0 g, 0.21 mol) which had been dehydrated and deaerated, followed by charging of argon gas. A small amount of iodine was slowly added to the mixture. 2-Ethylbutylbromide (29.5 g, 0.18 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 n-hexyltrichlorosilane (38 g, 0.17 mol) in anhydrous tetrahydrofuran (100 mL) in another reactor which had been dehydrated and deaerated, followed by charging of argon gas, at 60° C.-70° 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 60° C.-70° 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 (5.0 g, 0.21 mol) which had been dehydrated and deaerated, followed by charging of argon gas. A small amount of iodine was slowly added to the mixture. 3-Methylbutylbromide (25 g, 0.17 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 n-hexyltrichlorosilane (38 g, 0.17 mol) in anhydrous tetrahydrofuran (100 mL) in another reactor which had been dehydrated and deaerated, followed by charging of argon gas, at 60° C.-70° 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 60° C.-70° 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 (5.0 g, 0.21 mol) which had been dehydrated and deaerated, followed by charging of argon gas. A small amount of iodine was slowly added to the mixture. 3-Methylbutylbromide (25 g, 0.17 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 n-hexyltrichlorosilane (38 g, 0.17 mol) in anhydrous tetrahydrofuran (100 mL) in another reactor which had been dehydrated and deaerated, followed by charging of argon gas, at 60° C.-70° 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 60° C.-70° 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 diethyl ether (125 mL) was put into a reactor with magnesium (5.0 g, 0.21 mol) which had been dehydrated and deaerated, followed by charging of argon gas. A small amount of iodine was slowly added to the mixture. i-Butylbromide (25 g, 0.18 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 n-hexyltrichlorosilane (64 g, 0.25 mol) in anhydrous diethyl ether (50 mL)/anhydrous tetrahydrofuran (50 mL) in another reactor which had been dehydrated and deaerated, followed by charging of argon gas, at 50° C.-60° 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 50° C.-60° 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