참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Isopropanol | HCID 3776 | — |
| 반응물 | 1-Bromo-4-fluorobenzene | HCID 9993 | — |
| 반응물 | Trichloro(chloromethyl)silane | HCID 15258 | — |
| 반응물 | Magnesium | HCID 5462224 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | Chloro(chloromethyl)[bis(4-fluorophenyl)]silane | HCID 13392398 | 61% |
반응 단계
A suspension of 7.0 g (0.288 mol) of magnesium turnings in 50 ml of ether was stirred under nitrogen while a solution of 50.2 g (0.287 mol) of 4-bromofluorobenzene in 200 ml of ether was added dropwise at a rate that maintained gentle reflux. After another 2 hours at reflux, the mixture was chilled in ice and a solution of 12.0 ml (0.096 mol) of chloromethyltrichlorosilane in 30 ml of ether was added dropwise. The resulting mixture was refluxed for 4 hours, chilled in ice, treated with a solution of 7.5 ml of isopropanol in 20 ml of ether, stirred 5 minutes, and filtered. The filtrate was evaporated to leave a viscous oil that was stirred with hexanes to give a slurry. Filtration under nitrogen and evaporation of the filtrate left a mobile oil that was distilled to give 17.6 g (61%) of the title compound: bp 100°-140° (0.1 mm); nmr (CDCl3) 3.3 (2H, s), 7.1 (4H, t), 7.7 (4H, d of d).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US04510136 |
|---|
| 출처 데이터셋 | uspto-grants-1985_04 |
|---|
| ORD ID | ord-2bf285dc180946349040e574b47bfa9c |
|---|
| 출처 메모 | uspto-grants-1985_04 |
|---|