참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Iodine | HCID 807 | — |
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Chlorocyclohexane | HCID 10952 | — |
| 반응물 | Isobutyltrimethoxysilane | HCID 87622 | — |
| 반응물 | Magnesium | HCID 5462224 | — |
| 용매 | tert-Butyl methyl ether | HCID 15413 | — |
| 생성물 | Silane, cyclohexyldimethoxy(2-methylpropyl)- | HCID 14513104 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US04958041 |
|---|
| 출처 데이터셋 | uspto-grants-1990_09 |
|---|
| ORD ID | ord-a26ad30f1f404dbca25184fe25d06c96 |
|---|
| 출처 메모 | uspto-grants-1990_09 |
|---|