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Hydrochloric Acid → 4-(4-Ethyl-piperazin-1-yl)-2,6-difluoro-phenylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | N-Boc-4-(4-ethyl-piperazin-1-yl)-2,6-difluoro-phenylamine | HCID 59244991 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-(4-Ethyl-piperazin-1-yl)-2,6-difluoro-phenylamine | HCID 59244379 | 78.4% |
反応手順
To a solution of N-Boc-4-(4-ethyl-piperazin-1-yl)-2,6-difluoro-phenylamine (2.4 g, 7.03 mmol) obtained in Step B in ethyl acetate (20 ml), 6M−HCl aqueous solution (10 ml) was added, followed by stirring at room temperature for 1 hour. To this, 5M-NaOH aqueous solution was added to adjust the pH to 8, followed by extraction with ethyl acetate (50 ml×2). The organic layer was dried over sodium sulfate, and the solvent was distilled off under reduced pressure. This was purified by silica gel column chromatography (dichloromethane/methanol=50/1 to 20/1), followed by further dissolution in a minimum amount of dichloromethane. n-Hexane was added, and an oily component was removed, to obtain the desired compound as a brown solid (1.33 g, 78%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08022205B2 |
| 出典データセット | uspto-grants-2011_09 |
| ORD ID | ord-3fe10de404714d22bf21126f9d92f609 |
| 出典メモ | uspto-grants-2011_09 |