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Potassium Carbonate → 4-Acetyl-1-(3-aminopropyl)-4-phenylpiperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Bromopropylamine hydrobromide | HCID 78701 | — |
| 反応物 | 4-Acetyl-4-phenylpiperidine | HCID 101521 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 4-Acetyl-1-(3-aminopropyl)-4-phenylpiperidine | HCID 10587447 | 40% |
反応手順
4-Acetyl-4-phenylpiperidine (1.53 g, 7.50 mmol, 1.00 equiv, Aldrich), 3-bromopropylamine hydrobromide (1.64 g, 7.50 mmol, 1.00 equiv) and potassium carbonate (1.24 g, 9.00 mmol, 1.20 equiv) were stirred in refluxing 1,4-dioxane (50 mL) for 12 hours. After removal of dioxane, water (50 mL) was added and the pH was adjusted to 11-12 by addition of 1 N aqueous NaOH. The mixture was extracted with CH2Cl2 (100 mL+3×50 mL). The combined organic solutions were dried over MgSO4 and concentrated. The residue was purified by flash chromatography (EtOAc-MeOH-Et3N 100:40:20) to give 780 mg (40%) of colorless oil, which was characterized spectroscopically.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06608086B2 |
| 出典データセット | uspto-grants-2003_08 |
| ORD ID | ord-9c1ed14dcbc6423e8cf989edca1041ea |
| 出典メモ | uspto-grants-2003_08 |