関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Chlorocyclohexane | HCID 10952 | — |
| 反応物 | Isobutyltrimethoxysilane | HCID 87622 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 溶媒 | tert-Butyl methyl ether | HCID 15413 | — |
| 生成物 | Silane, cyclohexyldimethoxy(2-methylpropyl)- | HCID 14513104 | — |
反応手順
Under an inert gas, 24.3 g magnesium chips (1.0 mol) were combined with about 10 ml methyl-tert-butylether, an iodine crystal and 3.6 g cyclohexylchloride (0.03 mol). To start the reaction, a solution of 152.0 g isobutyltrimethoxysilane (0.85 mol) and 115.0 g cyclohexylchloride (0.97 mol) in 130 ml methyl-tert-butylether was added dropwise, with stirring, to the first mixture at a rate to maintain a moderate reflux. At the end of this addition, the reaction was allowed to reflux for two more hours. After cooling the reaction mixture, 4.8 g methanol (0.15 mol) was added, stirred for a few minutes and then the precipitate was removed by filtration. The filter cake was washed with several portions of methyl-tert-butylether. The solvent was evaporated from the combined filtrates by water vacuum. The remaining residue consisted of 192.5 g (98.4% of the theoretical yield) isobutylcyclohexyldimethoxysilane which had a purity of 98% according to GC. Isobutyldicyclohexylmethoxysilane was not detected by GC.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04958041 |
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| 出典データセット | uspto-grants-1990_09 |
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| ORD ID | ord-a26ad30f1f404dbca25184fe25d06c96 |
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| 出典メモ | uspto-grants-1990_09 |
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