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Acetyl chloride → 4'-Chloro-2'-fluoroacetanilide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 4-Chloro-2-fluoroaniline | HCID 93898 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4'-Chloro-2'-fluoroacetanilide | HCID 853174 | — |
反応手順
Acetyl chloride (24.2 mL, 0.34 mol) is added slowly to a solution of 4-chloro-2-fluoroaniline (49.4 g, 0.34 mol), and triethylamine (47 mL, 0.34 mol) in tetrahydrofuran while maintaining the reaction mixture temperature below 20° C. After the addition is complete, the reaction mixture is stirred overnight at room temperature, and poured into ethyl acetate. The organic solution is washed sequentially with water and brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to obtain an off-white solid. A mixture of the solid in ethanol is stirred for several minutes, and filtered to give the title product as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05726126 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-2e03a241be2b4b53bf88ccfacb21967f |
| 出典メモ | uspto-grants-1998_03 |