化工社化工社 化学情報印刷レポート · 研究参考用
1,2-Dichloroethane → 1-(4-Bromo-2-fluorophenyl)-3-chloro-1-propanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | 4-Bromo-2-fluorobenzoyl chloride | HCID 2734026 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 生成物 | 1-(4-Bromo-2-fluorophenyl)-3-chloro-1-propanone | HCID 59473827 | 68% |
反応手順
To a stirred suspension of aluminum trichloride (153 g, 1.15 mol) in DCE (1000 mL) was added a solution of 144b (271 g, 1.14 mol) in DCE (1000 mL) at 0° C. See FIG. 3. Ethylene gas was bubbled through the dark suspension for 3 h until the acid chloride was consumed. The reaction mixture was then stirred at RT overnight, cooled to 0° C., and quenched with 4M HCl (500 mL). The organic phase was separated and washed with brine (100 mL), dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The crude residue was purified by column chromatography (PE/EA=30 to 10:1) to give 1-(4-bromo-2-fluorophenyl)-3-chloropropan-1-one 144c (210 g, 68%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09326985B2 |
| 出典データセット | uspto-grants-2016_05 |
| ORD ID | ord-9946ceff88c245b994c6a22182dd4693 |
| 出典メモ | uspto-grants-2016_05 |