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Hydrochloric Acid → 4-Chloro-2-fluoro-3-iodoaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | N-(4-chloro-2-fluoro-3-iodophenyl)acetamide | HCID 68997639 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-Chloro-2-fluoro-3-iodoaniline | HCID 68823320 | — |
反応手順
To a mixture of N-(4-chloro-2-fluoro-3-iodophenyl)acetamide (20.0 g, 64 mmol) in MeOH (80 mL) is added concentrated HCl (60 mL). The mixture is stirred at reflux for 18 hours before cooling to room temperature and removal of the solvent under reduced pressure while maintaining the water bath below 45° C. The residue is cooled with an ice bath and a 1N NaOH solution is added to adjust the pH between 9 and 10. The aqueous phase is extracted with ether and dried over MgSO4. The solvent is removed and the residue is purified through a flash chromatographic column with a gradient of hexanes/ether to give 4-chloro-2-fluoro-3-iodoaniline.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08586782B2 |
| 出典データセット | uspto-grants-2013_11 |
| ORD ID | ord-3dcf60b1c1024b87a6cc0c73f9076183 |
| 出典メモ | uspto-grants-2013_11 |