dichloro-methyl-phenylsilane

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

Procedure: Methylphenyl dichlorosilane (765 g; 4.0 mol.) and the same amount of diethyl ether were introduced into a four-necked flask of 2 liters volume equipped with a stirring machine, a reflux condenser, a thermometer and a dropping funnel, followed by stirring the mixture, dropwise adding 36 g (2.0 mol.) of water through the dropping funnel over five hours under nitrogen atmosphere, and then refluxing the mixture for an additional three hours. After refluxing the mixture, ether was distilled off and the starting material, methylphenyl dichlorosilane (184 g; 0.96 mol.) was recovered by distilling the reaction mixture in vacuo to obtain 220 g (0.67 mol.) of 1,3-dimethyl-1,3-diphenyl dichlorodisiloxane. Boiling Point=135°-138° C./2 mmHg. equipped with a stirring machine, a reflux condenser refluxing the mixture for an additional three hours was distilled off by distilling the reaction mixture in vacuo

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

Procedure: Methylphenyl dichlorosilane (765 g; 4.0 mol.) and the same amount of diethyl ether were introduced into a four-necked flask of 2 liters volume equipped with a stirring machine, a reflux condenser, a thermometer and a dropping funnel, followed by stirring the mixture, dropwise adding 36 g (2.0 mol.) of water through the dropping funnel over five hours under nitrogen atmosphere, and then refluxing the mixture for an additional three hours. After refluxing the mixture, ether was distilled off and the starting material, methylphenyl dichlorosilane (184 g; 0.96 mol.) was recovered by distilling the reaction mixture in vacuo to obtain 220 g (0.67 mol.) of 1,3-dimethyl-1,3-diphenyl dichlorodisiloxane. Boiling Point=135°-138° C./2 mmHg. equipped with a stirring machine, a reflux condenser refluxing the mixture for an additional three hours was distilled off by distilling the reaction mixture in vacuo

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

Procedure: In a 500 mL two neck rb flask equipped with a reflux condenser, a Teflon covered magnetic stirring bar and a rubber septum was placed active magnesium powder (9.6 g, 0.4 mol), methylphenyldichlorosilane (38.2 g, 0.2 mol) and THF (300 mL). The reflux condenser was connected to a refrigeration unit. Ethylene glycol cooled to -20° C. was circulated through the reflux condenser. 1,3-Butadiene (15.1 g, 0.28 mol) was condensed at -78° C. into a volumetric flask which was sealed with a rubber septum. The 1,3-butadiene was transferred into the reaction via a cannula. The reaction mixture was stirred at rt for 24 h. Ether (2×100 mL) was added. The organic solution was decanted from the magnesium chloride salts. These were transferred to a sintered glass funnel and were washed with ether (100 mL). The combined organic solution was washed with water (2×50 mL), dried over anhydrous magnesium sulfate, filtered and the volatile solvents removed by evaporation under reduced pressure. The residue was purified by distillation through a 10 cm vacuum jacketed Vigreux column. The expected compound, bp 105°-107° C., 5 mm Hg, 42% yield, was collected. condensed at -78° C. into a volumetric flask which was sealed with a rubber septum The organic solution was decanted from the magnesium chloride salts These were transferred to a sintered glass funnel were washed with ether (100 mL) The combined organic solution was washed with water (2×50 mL) dried over anhydrous magnesium sulfate filtered the volatile solvents removed by evaporation under reduced pressure The residue was purified by distillation through a 10 cm vacuum The expected compound, bp 105°-107° C., 5 mm Hg, 42% yield, was collected

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

Procedure: In a 500 mL two neck rb flask equipped with a reflux condenser, a Teflon covered magnetic stirring bar and a rubber septum was placed active magnesium powder (9.6 g, 0.4 mol), methylphenyldichlorosilane (38.2 g, 0.2 mol) and THF (300 mL). The reflux condenser was connected to a refrigeration unit. Ethylene glycol cooled to -20° C. was circulated through the reflux condenser. 1,3-Butadiene (15.1 g, 0.28 mol) was condensed at -78° C. into a volumetric flask which was sealed with a rubber septum. The 1,3-butadiene was transferred into the reaction via a cannula. The reaction mixture was stirred at rt for 24 h. Ether (2×100 mL) was added. The organic solution was decanted from the magnesium chloride salts. These were transferred to a sintered glass funnel and were washed with ether (100 mL). The combined organic solution was washed with water (2×50 mL), dried over anhydrous magnesium sulfate, filtered and the volatile solvents removed by evaporation under reduced pressure. The residue was purified by distillation through a 10 cm vacuum jacketed Vigreux column. The expected compound, bp 105°-107° C., 5 mm Hg, 42% yield, was collected. condensed at -78° C. into a volumetric flask which was sealed with a rubber septum The organic solution was decanted from the magnesium chloride salts These were transferred to a sintered glass funnel were washed with ether (100 mL) The combined organic solution was washed with water (2×50 mL) dried over anhydrous magnesium sulfate filtered the volatile solvents removed by evaporation under reduced pressure The residue was purified by distillation through a 10 cm vacuum The expected compound, bp 105°-107° C., 5 mm Hg, 42% yield, was collected

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

Procedure: The procedure of Reference Example 2 was followed, but using a mixture of 60 g methylphenyldichlorosilane and 90 g dimethyldichlorosilane in place of the methylphenyldichlorosilane used in Reference Example 2. The product was a methylphenylsilanedimethylsilane copolymer with an average molecular weight of 40,000 and a softening point of 125 degrees Centigrade. a softening point of 125 degrees Centigrade

Conditions: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a round flask (internal volume: 1000 ml) equipped with a three-way stopcock, 90 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 114.7 g (0.6 mol) of methylphenyldichlorosilane purified by distillation and 35.4 g (0.2 mol) of phenyldichlorosilane 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, 2000 ml of 1N (=μmol/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 methylphenyldichlorosilane-phenyldichlorosilane copolymer (the former/the latter (molar ratio)=3/1) (weight-average molecular weight: 4000). 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, 2000 ml of 1N (=μmol/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

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

Procedure: In a 500 mL two neck rb flask equipped with a reflux condenser, a Teflon covered magnetic stirring bar and a rubber septum was placed magnesium powder (9.6 g, 0.4 mol), methylphenyldichlorosilane (38.2 g, 0.2 mol) and THF (300 mL). The reflux condenser was connected to a refrigeration unit. Isopropyl alcohol cooled to -20° C. was circulated through the reflux condenser. 1,3-Butadiene (15.1 g, 0.28 mol) was condensed at -78° C. into a volumetric flask which was sealed with a rubber septum. The 1,3-butadiene was transferred into the reaction via a cannula. The reaction mixture was stirred at rt for 24 h. Ether (2×100 mL) was added. The organic solution was decanted from the magnesium chloride salts. These were transferred to a sintered glass funnel and were washed with ether (100 mL). The combined organic solution was washed with water (2×50 mL), dried over anhydrous magnesium sulfate, filtered and the volatile solvents removed by evaporation under reduced pressure. The residue was purified by distillation through a 10 cm vacuum jacketed Vigreux column. The expected compound (boiling point 85°-87° C. at 4 mm Hg, 22.6 g, 65 % yield) was collected. condensed at -78° C. into a volumetric flask which was sealed with a rubber septum The organic solution was decanted from the magnesium chloride salts These were transferred to a sintered glass funnel were washed with ether (100 mL) The combined organic solution was washed with water (2×50 mL) dried over anhydrous magnesium sulfate filtered the volatile solvents removed by evaporation under reduced pressure The residue was purified by distillation through a 10 cm vacuum

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

Procedure: In a 500 mL two neck rb flask equipped with a reflux condenser, a Teflon covered magnetic stirring bar and a rubber septum was placed active magnesium powder (9.6 g, 0.4 mol), methylphenyldichlorosilane (38.2 g, 0.2 mol) and THF (300 mL). The reflux condenser was connected to a refrigeration unit. Ethylene glycol cooled to -20° C. was circulated through the reflux condenser. 1,3-Butadiene (15.1 g, 0.28 mol) was condensed at -78° C. into a volumetric flask which was sealed with a rubber septum. The 1,3-butadiene was transferred into the reaction via a cannula. The reaction mixture was stirred at rt for 24 h. Ether (2×100 mL) was added. The organic solution was decanted from the magnesium chloride salts. These were transferred to a sintered glass funnel and were washed with ether (100 mL). The combined organic solution was washed with water (2×50 mL), dried over anhydrous magnesium sulfate, filtered and the volatile solvents removed by evaporation under reduced pressure. The residue was purified by distillation through a 10 cm vacuum jacketed Vigreux column. The expected compound, bp 105°-107° C., 5 mm Hg, 42% yield, was collected. condensed at -78° C. into a volumetric flask which was sealed with a rubber septum The organic solution was decanted from the magnesium chloride salts These were transferred to a sintered glass funnel were washed with ether (100 mL) The combined organic solution was washed with water (2×50 mL) dried over anhydrous magnesium sulfate filtered the volatile solvents removed by evaporation under reduced pressure The residue was purified by distillation through a 10 cm vacuum The expected compound, bp 105°-107° C., 5 mm Hg, 42% yield, was collected

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

Procedure: Methylphenyl dichlorosilane (765 g; 4.0 mol.) and the same amount of diethyl ether were introduced into a four-necked flask of 2 liters volume equipped with a stirring machine, a reflux condenser, a thermometer and a dropping funnel, followed by stirring the mixture, dropwise adding 36 g (2.0 mol.) of water through the dropping funnel over five hours under nitrogen atmosphere, and then refluxing the mixture for an additional three hours. After refluxing the mixture, ether was distilled off and the starting material, methylphenyl dichlorosilane (184 g; 0.96 mol.) was recovered by distilling the reaction mixture in vacuo to obtain 220 g (0.67 mol.) of 1,3-dimethyl-1,3-diphenyl dichlorodisiloxane. Boiling Point=135°-138° C. /2 mmHg. equipped with a stirring machine, a reflux condenser refluxing the mixture for an additional three hours was distilled off by distilling the reaction mixture in vacuo

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

Procedure: Methylphenyl dichlorosilane (765 g; 4.0 mol.) and the same amount of diethyl ether were introduced into a four-necked flask of 2 liters volume equipped with a stirring machine, a reflux condenser, a thermometer and a dropping funnel, followed by stirring the mixture, dropwise adding 36 g (2.0 mol.) of water through the dropping funnel over five hours under nitrogen atmosphere, and then refluxing the mixture for an additional three hours. After refluxing the mixture, ether was distilled off and the starting material, methylphenyl dichlorosilane (184 g; 0.96 mol.) was recovered by distilling the reaction mixture in vacuo to obtain 220 g (0.67 mol.) of 1,3-dimethyl-1,3-diphenyl dichlorodisiloxane. Boiling Point=135°-138° C./2 mmHg. equipped with a stirring machine, a reflux condenser refluxing the mixture for an additional three hours was distilled off by distilling the reaction mixture in vacuo

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

Procedure: In a 500 mL two neck rb flask equipped with a reflux condenser, a Teflon covered magnetic stirring bar and a rubber septum was placed active magnesium powder (9.6 g, 0.4 mol), methylphenyldichlorosilane (38.2 g, 0.2 mol) and THF (300 mL). The reflux condenser was connected to a refrigeration unit. Ethylene glycol cooled to -20° C. was circulated through the reflux condenser. 1,3-Butadiene (15.1 g, 0.28 mol) was condensed at -78° C. into a volumetric flask which was sealed with a rubber septum. The 1,3-butadiene was transferred into the reaction via a cannula. The reaction mixture was stirred at rt for 24 h. Ether (2×100 mL) was added. The organic solution was decanted from the magnesium chloride salts. These were transferred to a sintered glass funnel and were washed with ether (100 mL). The combined organic solution was washed with water (2×50 mL), dried over anhydrous magnesium sulfate, filtered and the volatile solvents removed by evaporation under reduced pressure. The residue was purified by distillation through a 10 cm vacuum jacketed Vigreux column. The expected compound, bp 105°-107° C., 5 mm Hg, 42% yield, was collected. condensed at -78° C. into a volumetric flask which was sealed with a rubber septum The organic solution was decanted from the magnesium chloride salts These were transferred to a sintered glass funnel were washed with ether (100 mL) The combined organic solution was washed with water (2×50 mL) dried over anhydrous magnesium sulfate filtered the volatile solvents removed by evaporation under reduced pressure The residue was purified by distillation through a 10 cm vacuum The expected compound, bp 105°-107° C., 5 mm Hg, 42% yield, was collected