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Acetone → 3-(4-Phenylpiperazin-1-yl)propan-1-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | 1-Phenylpiperazine | HCID 7096 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Bromopropylamine hydrobromide | HCID 78701 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3-(4-Phenylpiperazin-1-yl)propan-1-amine | HCID 261297 | 56.3% |
反応手順
4-Phenylpiperazine (5.00 g, 30.8 mmol, 1.00 equiv, Aldrich), 3-bromopropylamine hydrobromide (8.09 g, 37.0 mmol, 1.20 equiv) and potassium carbonate (8.51 g, 61.6 mmol, 2.00 equiv) were stirred in refluxing acetone (200 mL) and EtOH (40 mL) for 14 hours. After removal of the solvents, water (250 mL) was added and the pH was adjusted to 11-12 by addition of 1 N aqueous NaOH. The mixture was extracted with CH2Cl2 (4×250 mL). The combined organic solutions were dried over MgSO4 and concentrated. The residue was purified by flash chromatography (SiO2, CHCl3-MeOH-NH (2 M in MeOH) 100:10:5 to 100:20:10) to give 3.80 g (56%) of yellow 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-c1ed6536eb454aa1a3021a9fd5114f59 |
| 出典メモ | uspto-grants-2003_08 |