HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Carbonate → 4-Acetyl-1-(3-aminopropyl)-4-phenylpiperidine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 3-Bromopropylamine hydrobromide | HCID 78701 | — |
| Edukt | 4-Acetyl-4-phenylpiperidine | HCID 101521 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | 4-Acetyl-1-(3-aminopropyl)-4-phenylpiperidine | HCID 10587447 | 40% |
Reaktionsschritte
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 1N 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.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06211198B1 |
| Quelldatensatz | uspto-grants-2001_04 |
| ORD ID | ord-6d7c7d93fb5f4da19e75f1fd2b63b7a6 |
| Quellennotiz | uspto-grants-2001_04 |