関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Cyclohexane | HCID 8078 | — |
| 反応物 | 1-Bromo-1,2,2-trifluoroethene | HCID 11730 | — |
| 反応物 | Chloro(4-ethoxyphenyl)dimethylsilane | HCID 14014482 | — |
| 反応物 | CID 53628100 | HCID 178418400 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | p-[(Trifluorovinyl)dimethylsilyl]phenetole | HCID 19706492 | 66.9% |
反応手順
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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05710102 |
|---|
| 出典データセット | uspto-grants-1998_01 |
|---|
| ORD ID | ord-3bc9fb260f91463c93e8c4ad1090e966 |
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| 出典メモ | uspto-grants-1998_01 |
|---|
