HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methylamine → (4E)-N-Methyl-5-(3-pyridyl)-4-penten-2-amine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methylamine | HCID 6329 | — |
| Edukt | (4E)-5-(3-Pyridyl)-4-pentene-2-ol p-Toluenesulfonate | HCID 87466987 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | (4E)-N-Methyl-5-(3-pyridyl)-4-penten-2-amine | HCID 10219654 | 51,6% |
Reaktionsschritte
A mixture of (4E)-5-(3-pyridyl)-4-penten-2-ol p-toluenesulfonate (5.60 g, 17.66 mmol), methylamine (100 mL, 40% solution in water), and ethyl alcohol (10 mL) was stirred at ambient temperature for 18 h. The resulting solution was extracted with chloroform (3×100 mL). The combined chloroform extracts were dried over sodium sulfate, filtered, and concentrated by rotary evaporation. The crude product was purified by column chromatography over aluminum oxide, eluting with ethyl acetate-methanol (7:3, v/v). Selected fractions were combined and concentrated by rotary evaporation, producing an oil. Further purification by vacuum distillation furnished 1.60 g (51.6%) of a colorless oil, bp 110-120° C. at 0.1 mm Hg.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06455554B1 |
| Quelldatensatz | uspto-grants-2002_09 |
| ORD ID | ord-049962c03a7946fea1744aacfd650ea0 |
| Quellennotiz | uspto-grants-2002_09 |