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1,3-Difluorobenzene → 4-Chloro-1-(2,4-difluorophenyl)butan-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,3-Difluorobenzene | HCID 9741 | — |
| 反応物 | 4-Chlorobutyryl chloride | HCID 78370 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Chloro-1-(2,4-difluorophenyl)butan-1-one | HCID 10331010 | 85.2% |
反応手順
255 g (1.81 mols) of 4-chlorobutyryl chloride are added dropwise to a mixture of 200 g (1.75 mols) of 1,3-difluorobenzene and 256 g (1.92 mols) of anhydrous aluminum chloride at room temperature, while stirring. The mixture is stirred at 30° C. for 4 hours and then poured onto 1,200 g of ice. 1,200 ml of methylene chloride are added, the organic phase is separated off, the aqueous phase is extracted with methylene chloride and the combined organic phases are washed with water, dried over sodium sulphate and concentrated by stripping off the solvent under reduced pressure. The residue which remains is distilled. 326 g (85% of theory) of 2,4-difluorophenyl 3-chloropropyl ketone are obtained in this manner.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04845116 |
| 出典データセット | uspto-grants-1989_07 |
| ORD ID | ord-c62facb23d654e3e81f07915e4d8f847 |
| 出典メモ | uspto-grants-1989_07 |