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Hydrochloric Acid → 4,4,4-Trifluoro-1-(3-chloro-4-methoxylphenyl)-1,3-butanedione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethyl trifluoroacetate | HCID 9794 | — |
| 反応物 | 3'-Chloro-4'-methoxyacetophenone | HCID 520857 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4,4,4-Trifluoro-1-(3-chloro-4-methoxylphenyl)-1,3-butanedione | HCID 12972728 | — |
反応手順
To stirred solution of 1-(3-chloro-4-methoxyphenyl)ethanone (2.2 g, 12 mmol) in DME was added ethyl trifluoroacetate (4.28 ml, 36 mmol) and sodium methoxide (4.25 g, 72 mmol), and the resulting reaction mixture was stirred at room temperature for 1 hour. EtOAc (200 ml) and water (50 ml) were added, and the pH of the aqueous layer was adjusted to 6 by addition of 1 N HCl solution. The organic layer was washed with brine (50 ml), dried over MgSO4, and concentrated in vacuo to give the title compound in quantitative yield. This was used for the next coupling step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06531492B1 |
| 出典データセット | uspto-grants-2003_03 |
| ORD ID | ord-bb16ff7b1ccb4c738b47374be0df0e0d |
| 出典メモ | uspto-grants-2003_03 |