HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → 4-[3-(Nicotinoylamino)propylthio]pyridine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 3-Pyridinecarbonyl chloride, hydrochloride (1:1) | HCID 88438 | — |
| Edukt | 4-(3-Aminopropylthio)pyridine dihydrochloride | HCID 19079259 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 4-[3-(Nicotinoylamino)propylthio]pyridine | HCID 15231489 | 75,8% |
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 methylene chloride (100 ml), 8.86 g (49.8 mmol) of nicotinoyl chloride hydrochloride 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=1:10) to obtain powder. The powder was washed with ether and dried to obtain the desired compound (8.50 g, yield: 75.8%, pale yellow powder).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05246948 |
| Quelldatensatz | uspto-grants-1993_09 |
| ORD ID | ord-2e39c2dcd2084984895ee85c814023f7 |
| Quellennotiz | uspto-grants-1993_09 |