bis(dimethylsilyloxy)-dimethylsilane

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a 1000 ml 3-necked flask was added 208.5 grams (1 mole) purified 1,1,3,3,5,5-hexamethyltrisiloxane prepared in Example 1, 153.3 grams (2.1 moles) of N-methylacetamide, 173.2 grams of toluene and about 120 ppm of platinum containing catalyst (as Pt) prepared in accordance with the teaching of U.S. Pat. No. 3,220,970 to Lamoreaux (hereinafter Lamoreaux catalyst). To the flask was attached a mechanical stirrer, a thermometer and a reflux condenser. The reaction mixture was heated at 100° C. for 20 hours and thereafter heated at 130° C. for 24 hours. At the end of the 44 hour period, analysis by infrared spectroscopy showed no Si--H present in the reaction mixture. The solvent was removed by distillation and the residue filtered through Celite R to give 317.5 grams (90.6% theoretical) of 1,5-bits (N-methylacetamido)-1,1,3,3,5,5-hexamethyltrisiloxane. To a 1000 ml 3-necked flask was added 208.5 grams (1 mole) prepared in accordance with the teaching of U.S heated at 130° C. for 24 hours At the end of the 44 hour period, analysis The solvent was removed by distillation the residue filtered through Celite R

反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Allyloxybenzophenone 1 (200 g, 840 mmol) was dissolved with warming in THF (150 mL, EM Science) and charged to an addition funnel placed on a 2 L four-necked flask equipped with a mechanical stirrer, reflux condenser and internal temperature probe under a dry air purge. To the reaction vessel was added 1,1,3,3-tetramethyldisiloxane (740 mL, 4.18 mol, Hanse Chemie) and THF (100 mL). The internal pot temperature was raised to 50° C., at which point chlorotris(triphenylphosphine) rhodium (“Wilkinson's catalyst”, 22 mg, 11 ppm based on mass of allyloxybenzophenone 1, Aldrich Chemcial) was added to the pot along with a portion (5 mL) of the 4-allyloxybenzophenone/THF solution. The internal reaction temperature was raised to 60° C., at which point the 4-allyloxybenzophenone solution was added to the reactor pot over the course of 45 min. The internal temperature of the reaction was held between 60-65° C. during the course of the addition, which is exothermic. After the addition was complete, the reaction was stirred at 60° C. for an additional 15 min., at which point no starting material was present by GC analysis. The reaction was allowed to cool to 35° C., and activated carbon (3 lab scoops, Aldrich Chemical) was added. The resulting slurry was stirred for 30 min., then filtered to yield a pale yellow solution. Solvent was removed from the product in vacuo to yield a yellow oil (329 g, 104% due to presence of ˜10 mol % 1,1,3,3,5,5-hexamethyltrisiloxane in the commercial grade 1,1,3,3-tetramethyldisiloxne starting material; i.e. the reaction is essentially quantitative). The product exhibited acceptable 1H, 13C and 29Si NMR, UV-Vis and FT-IR spectral characteristics. charged to an addition funnel placed on a 2 L four-necked flask equipped with a mechanical stirrer reflux condenser internal temperature probe under a dry air purge was added to the reactor pot over the course of 45 min The internal temperature of the reaction was held between 60-65° C. during the course of the addition, which After the addition to cool to 35° C. activated carbon (3 lab scoops, Aldrich Chemical) was added The resulting slurry was stirred for 30 min. filtered to yield a pale yellow solution Solvent was removed from the product in vacuo

反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Allyloxybenzophenone 1 (200 g, 840 mmol) was dissolved with warming in THF (150 mL, EM Science) and charged to an addition funnel placed on a 2 L four-necked flask equipped with a mechanical stirrer, reflux condenser and internal temperature probe under a dry air purge. To the reaction vessel was added 1,1,3,3-tetramethyldisiloxane (740 mL, 4.18 mol, Hanse Chemie) and THF (100 mL). The internal pot temperature was raised to 50° C., at which point chlorotris(triphenylphosphine) rhodium (“Wilkinson's catalyst”, 22 mg, 11 ppm based on mass of allyloxybenzophenone 1, Aldrich Chemical) was added to the pot along with a portion (5 mL) of the 4-allyloxybenzophenone/THF solution. The internal reaction temperature was raised to 60° C., at which point the 4-allyloxybenzophenone solution was added to the reactor pot over the course of 45 min. The internal temperature of the reaction was held between 60-65° C. during the course of the addition, which is exothermic. After the addition was complete, the reaction was stirred at 60° C. for an additional 15 min., at which point no starting material was present by GC analysis. The reaction was allowed to cool to 35° C., and activated carbon (3 lab scoops, Aldrich Chemical) was added. The resulting slurry was stirred for 30 min., then filtered to yield a pale yellow solution. Solvent was removed from the product in vacuo to yield a yellow oil (329 g, 104% due to presence of ˜10 mol % 1,1,3,3,5,5-hexamethyltrisiloxane in the commercial grade 1,1,3,3-tetramethyldisiloxane starting material; i.e. the reaction is essentially quantitative). The product exhibited acceptable 1H, 13C and 29Si NMR, UV-Vis and FT-IR spectral characteristics. charged to an addition funnel placed on a 2 L four-necked flask equipped with a mechanical stirrer reflux condenser internal temperature probe under a dry air purge was added to the reactor pot over the course of 45 min The internal temperature of the reaction was held between 60-65° C. during the course of the addition, which After the addition to cool to 35° C. activated carbon (3 lab scoops, Aldrich Chemical) was added The resulting slurry was stirred for 30 min. filtered to yield a pale yellow solution Solvent was removed from the product in vacuo

反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Allyloxybenzophenone 1 (200 g, 840 mmol) was dissolved with warming in THF (150 mL, EM Science) and charged to an addition funnel placed on a 2L four-necked flask equipped with a mechanical stirrer, reflux condenser and internal temperature probe under a dry air purge. To the reaction vessel was added 1,1,3,3-tetramethyldisiloxane (740 mL, 4.18 mol, Hanse Chemie) and THF (100 mL). The internal pot temperature was raised to 50° C., at which point chlorotris(triphenylphosphine) rhodium (“Wilkinson's catalyst”, 22 mg, 11 ppm based on mass of allyloxybenzophenone 1, Aldrich Chemcial) was added to the pot along with a portion (5 mL) of the 4-allyloxybenzophenone/THF solution. The internal reaction temperature was raised to 60° C., at which point the 4-allyloxybenzophenone solution was added to the reactor pot over the course of 45 min. The internal temperature of the reaction was held between 60–65° C. during the course of the addition, which is exothermic. After the addition was complete, the reaction was stirred at 60° C. for an additional 15 min., at which point no starting material was present by GC analysis. The reaction was allowed to cool to 35° C., and activated carbon (3 lab scoops, Aldrich Chemical) was added. The resulting slurry was stirred for 30 min., then filtered to yield a pale yellow solution. Solvent was removed from the product in vacuo to yield a yellow oil (329 g, 104% due to presence of ˜10 mol % 1,1,3,3,5,5-hexamethyltrisiloxane in the commercial grade 1,1,3,3-tetramethyldisiloxne starting material; i.e. the reaction is essentially quantitative). The product exhibited acceptable 1H, 13C & 29Si NMR, UV-Vis and FT-IR spectral characteristics. charged to an addition funnel equipped with a mechanical stirrer reflux condenser internal temperature probe under a dry air purge was added to the reactor pot over the course of 45 min The internal temperature of the reaction was held between 60–65° C. during the course of the addition, which After the addition to cool to 35° C. activated carbon (3 lab scoops, Aldrich Chemical) was added The resulting slurry was stirred for 30 min. filtered to yield a pale yellow solution Solvent was removed from the product in vacuo

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a 1000 ml 3-necked flask was added 208.5 grams (1 mole) purified 1,1,3,3,5,5-hexamethyltrisiloxane prepared in Example 1, 153.3 grams (2.1 moles) of N-methylacetamide, 173.2 grams of toluene and about 120 ppm of platinum containing catalyst (as Pt) prepared in accordance with the teaching of U.S. Pat. No. 3,220,970 to Lamoreaux (hereinafter Lamoreaux catalyst). To the flask was attached a mechanical stirrer, a thermometer and a reflux condenser. The reaction mixture was heated at 100° C. for 20 hours and thereafter heated at 130° C. for 24 hours. At the end of the 44 hour period, analysis by infrared spectroscopy showed no Si--H present in the reaction mixture. The solvent was removed by distillation and the residue filtered through Celite R to give 317.5 grams (90.6% theoretical) of 1,5-bits (N-methylacetamido)-1,1,3,3,5,5-hexamethyltrisiloxane. To a 1000 ml 3-necked flask was added 208.5 grams (1 mole) prepared in accordance with the teaching of U.S heated at 130° C. for 24 hours At the end of the 44 hour period, analysis The solvent was removed by distillation the residue filtered through Celite R