참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Cyclohexane | HCID 8078 | — |
| 반응물 | 1-Bromo-1,2,2-trifluoroethene | HCID 11730 | — |
| 반응물 | Chloro(4-ethoxyphenyl)dimethylsilane | HCID 14014482 | — |
| 반응물 | CID 53628100 | HCID 178418400 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | p-[(Trifluorovinyl)dimethylsilyl]phenetole | HCID 19706492 | 66.9% |
반응 단계
A -30° C. solution of bromotrifluoroethylene (7.15 g, 0.044 mol) in ether is treated with p-(chlorodimethylsilyl)phenetole (9.54 g, 0.044 mol), cooled to -65° C., treated dropwise with a 1.3M solution of sec-butyllithium in cyclohexane (34.2 mL, 0.044 mol) while maintaining the temperature below -60° C., stirred at -65° C. for 5 hours, stirred at room temperature overnight, cooled to 0° C., treated with dilute hydrochloric acid, and diluted with ether. The organic phase is separated, washed with brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to obtain a residue which is distilled to give the title product as a clear liquid (7.66 g, bp 84°-92° C./0.8 mm Hg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05710102 |
|---|
| 출처 데이터셋 | uspto-grants-1998_01 |
|---|
| ORD ID | ord-3bc9fb260f91463c93e8c4ad1090e966 |
|---|
| 출처 메모 | uspto-grants-1998_01 |
|---|
