化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Hydroxide → 1-Amino-5-fluoronaphthalene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-Fluoro-5-nitronaphthalene | HCID 21730284 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-Amino-5-fluoronaphthalene | HCID 21730289 | 81.2% |
反応手順
A solution of compound 208A (62 mg, 0.32 mmol) in 1 mL EtOH containing 0.1 mL 12 N HCl was heated to reflux. Iron powder (62 mg, 1.11 mmol) was added in small portions and heating was continued for 2 h. The mixture was cooled, neutralized with 1 N NaOH solution and the aqueous layer was extracted with CH2Cl2. The combined organic phases were dried over MgSO4 and concentrated in vacuo to leave a residue which was purified by flash chromatography on silica gel eluting with 40 to 80% EtOAc in hexanes to give 42 mg (0.26 mmol, 80%) of compound 208B as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06953679B2 |
| 出典データセット | uspto-grants-2005_10 |
| ORD ID | ord-77a22b4aaa9c49309bfa7e3fda7fe745 |
| 出典メモ | uspto-grants-2005_10 |