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Potassium Carbonate → 1,3-Dichloro-5-(3,3,3-trifluoroprop-1-en-2-yl)benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3,3,3-Trifluoropropene | HCID 12672 | — |
| 反応物 | 3,5-Dichlorophenylboronic acid | HCID 2734331 | — |
| 触媒 | HCID 178418476 | HCID 178418476 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1,3-Dichloro-5-(3,3,3-trifluoroprop-1-en-2-yl)benzene | HCID 23159823 | — |
反応手順
3,3,3-Trifluoropropene (3.2 g), potassium carbonate (4.6 g) and bis-(triphenylphosphine)-palladium chloride (0.2 g) is added to a solution of 3,5-dichlorophenylboronic acid in THF (20 ml) under nitrogen. After 3 hours at reflux, the reaction is quenched with ethyl acetate (50 ml) and water (50 ml). The organic phase is then extracted with water and with a saturated aqueous solution of NaCl, dried over Na2SO4 and concentrated in vacuo. The crude product is purified on silica gel (35×45 mm) using heptane (150 ml) as eluant to yield 1,3-dichloro-5-(1-trifluoromethyl-vinyl)-benzene (2.7 g), as a colorless oil. MS (HPLC/MS): no ionisation. Retention time: 5.10 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08653116B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-0ce6ebe3c44b4fac9a3a3d6c739dec98 |
| 出典メモ | uspto-grants-2014_02 |