“…No yield was given. 4 ) This also contrasts with the results using AlMe 3 , where protracted reflux or sealed-tube furnace heating regimes were employed.…”
Section: Synthesismentioning
confidence: 56%
“…The yield of 2 from route a (Scheme 1) was half of this, although higher temperatures, a more homogeneous starting material (Me 2 SiO) 4 , and a longer reaction time were employed. It would appear that the siloxane cleavage reaction may proceed under much less forcing conditions than were hitherto assumed.…”
Section: Synthesismentioning
confidence: 97%
“…It would appear that the siloxane cleavage reaction may proceed under much less forcing conditions than were hitherto assumed. (A more recently reported reaction of (Me 2 SiO) 4 with AlCl 3 did proceed at room temperature, but a reaction time of 6 days was employed, and the isolated material was the product of incomplete depolymerization, 1. No yield was given.…”
Section: Synthesismentioning
confidence: 99%
“…In the case of aluminum alkyls, the groups of Barron 1 and Ittel 2 have thoroughly investigated the area, and crystallographically characterized the dimeric siloxide product of full depolymerization, [{Me 3 SiOAlMe 2 } 2 ], 1,2 as well as many other examples and intermediate stages. 3,4 However, in these studies, clean products were most frequently available by ring-opening of small oligomeric cyclosiloxanes, such as (Me 2 SiO) 3 or (Me 2 SiO) 4 . Also, conditions were aggressive: either a 4 day toluene reflux or a 24 h heating of neat regents at 180…”
Reaction of AlCl 3 with {Me 2 SiO} n (Dow-Corning high-vacuum grease) at an Al : Si ratio of 1 : 1 in hexane at room temperature yielded a large crop of colorless crystals of [{ClSiMe 2 OAlCl 2 } 2 ], which were characterized by single-crystal X-ray diffraction and NMR. These crystals hydrolyzed on an aluminum surface to give a coating of silicone oil interspersed with particles of [Al(OH 2 ) 6 ]Cl 3 , as determined by powder X-ray diffraction and X-ray photoelectron spectrometry.
“…No yield was given. 4 ) This also contrasts with the results using AlMe 3 , where protracted reflux or sealed-tube furnace heating regimes were employed.…”
Section: Synthesismentioning
confidence: 56%
“…The yield of 2 from route a (Scheme 1) was half of this, although higher temperatures, a more homogeneous starting material (Me 2 SiO) 4 , and a longer reaction time were employed. It would appear that the siloxane cleavage reaction may proceed under much less forcing conditions than were hitherto assumed.…”
Section: Synthesismentioning
confidence: 97%
“…It would appear that the siloxane cleavage reaction may proceed under much less forcing conditions than were hitherto assumed. (A more recently reported reaction of (Me 2 SiO) 4 with AlCl 3 did proceed at room temperature, but a reaction time of 6 days was employed, and the isolated material was the product of incomplete depolymerization, 1. No yield was given.…”
Section: Synthesismentioning
confidence: 99%
“…In the case of aluminum alkyls, the groups of Barron 1 and Ittel 2 have thoroughly investigated the area, and crystallographically characterized the dimeric siloxide product of full depolymerization, [{Me 3 SiOAlMe 2 } 2 ], 1,2 as well as many other examples and intermediate stages. 3,4 However, in these studies, clean products were most frequently available by ring-opening of small oligomeric cyclosiloxanes, such as (Me 2 SiO) 3 or (Me 2 SiO) 4 . Also, conditions were aggressive: either a 4 day toluene reflux or a 24 h heating of neat regents at 180…”
Reaction of AlCl 3 with {Me 2 SiO} n (Dow-Corning high-vacuum grease) at an Al : Si ratio of 1 : 1 in hexane at room temperature yielded a large crop of colorless crystals of [{ClSiMe 2 OAlCl 2 } 2 ], which were characterized by single-crystal X-ray diffraction and NMR. These crystals hydrolyzed on an aluminum surface to give a coating of silicone oil interspersed with particles of [Al(OH 2 ) 6 ]Cl 3 , as determined by powder X-ray diffraction and X-ray photoelectron spectrometry.
“…The title complex (I) was isolated as a minor product from the recrystallization of (η 5 -C 5 H 5 )Fe(CO) 2 Ga( s Mes)Cl (Bunn NR, Aldridge S, unpublished results; s Mes = 2, 4, 6-t Bu 3 C 6 H 3 ) from toluene solution in the presence of adventitious silicone grease. The structure of the trigallasiloxane core ( Fig.…”
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