HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → 4-[3-(2-Thenoylamino)propylthio]pyridine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 2-Thiophenecarbonyl chloride | HCID 78928 | — |
| Edukt | 4-(3-Aminopropylthio)pyridine dihydrochloride | HCID 19079259 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 4-[3-(2-Thenoylamino)propylthio]pyridine | HCID 15231491 | 70,5% |
Reaktionsschritte
To a solution of 10.0 g (41.5 mmol) of 4-(3-aminopropylthio)pyridine dihydrochloride and 27.7 ml (200 mmol) of triethylamine in 100 ml of methylene chloride, 5.35 ml (50.0 mmol) of 2-thenoyl chloride was added under ice-cooling with stirring. The mixture was stirred at room temperature for 30 minutes. The reaction mixture was washed with a saturated aqueous solution of sodium bicarbonate and water and dried, and then the solvent was distilled off. The residue was purified by column chromatography (eluent: methanol/ethyl acetate=1:20) to obtain powder. The powder was recrystallized from methanol/ethyl acetate (=1:20) to obtain 8.05 g of the desired compound (yield: 70.5%, yellow prisms).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05246948 |
| Quelldatensatz | uspto-grants-1993_09 |
| ORD ID | ord-11093efb280540518b66f99ed8c2be55 |
| Quellennotiz | uspto-grants-1993_09 |