HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → 4-(3-(N-(2-thienylmethyl)amino)propylthio]pyridine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Methanesulfonyl chloride | HCID 31297 | — |
| Edukt | (2-Thienylmethyl)amine | HCID 34005 | — |
| Edukt | 4-(3-Hydroxypropylthio)pyridine | HCID 19079134 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 4-(3-(N-(2-thienylmethyl)amino)propylthio]pyridine | HCID 19079184 | 29,1% |
Reaktionsschritte
In 200 ml of methylene chloride were dissolved 10.34 g (61.1 mmol) of 4-(3-hydroxypropylthio)pyridine and 10.2 ml (73.3 mmol) of triethylamine, methanesulfonyl chloride [5.7 ml (73.3 mmol)] was added, and 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. Then the solvent was distilled off. To 8.05 g of the residue was added 3.3 ml (32.5 mmol) of 2-thiophenemethylamine. The mixture was heated at 80° C. for 3 hours. After cooling, the mixture was purified by column chromatography (eluent: chloroform/methanol=25:1) to obtain 2.5 g of the desired compound (yield: 29.1%, yellow oil).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05246948 |
| Quelldatensatz | uspto-grants-1993_09 |
| ORD ID | ord-80d6d35a6b1b4822a93a6f325c74f83a |
| Quellennotiz | uspto-grants-1993_09 |