関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | 2-Bromo-1,4-difluorobenzene | HCID 67862 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 生成物 | 1-(4-Bromo-2,5-difluorophenyl)ethan-1-one | HCID 9991653 | — |
反応手順
Acetyl chloride (17 ml) is slowly dropped into a stirred mixture of 1-bromo-2,5-difluorobenzene (30 g) and aluminium trichloride (53 g) heated at 60° C. and kept under argon. The reaction mixture is then stirred 90 minutes at 95° C. The mixture is cooled at 40° C. and carefully poured into crushed ice (400 g) and concentrated hydrochloric acid (35 ml). The resulting mixture is stirred a few minutes and then extracted with ethyl ether (2×250 ml). The ethereal solution is washed to neutral with brine, dried over sodium sulfate and the solvent is evaporated. The distillation of the oily residue gives 4'-bromo-2 ',5'-difluoroacetophenone (21.2 g) b.p. (0.05 mm)=60° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05786350 |
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| 出典データセット | uspto-grants-1998_07 |
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| ORD ID | ord-198b147a0184444fb062f6bd53d235b0 |
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| 出典メモ | uspto-grants-1998_07 |
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