Reaktion #6213

Reaktionsgleichung

2-(3-aminopropylthio)pyridine dihydrochloride

triethylamine

2-thenoyl-chloride

→

desired compound

Ausbeute 85.5%

2-[3-(thenoylamino)propylthio]pyridine

Ausbeute 85.5%

Lösungsmittel

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooling
2. 2
   workup.STIRRINGThe mixture was stirred at room temperature for 30 minutes
3. 3
   WaschenThe reaction mixture was washed with a saturated aqueous solution of sodium bicarbonate and water
4. 4
   Sonstigedried
5. 5
   workup.DISTILLATIONthe solvent was distilled off
6. 6
   SonstigeThe residue was purified by column chromatography (eluent: ethyl acetate)
7. 7
   Sonstigeto obtain powder
8. 8
   WaschenThe powder was washed with ether
9. 9
   Sonstigedried

Vorschrift

To a solution of 1.50 g (6.22 mmol) of 2-(3-aminopropylthio)pyridine dihydrochloride and 3.19 ml (22.9 mmol) of triethylamine in 60 ml of methylene chloride, 1.09 ml (7.46 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: ethyl acetate) to obtain powder. The powder was washed with ether and dried to obtain 1.48 g of the desired compound (yield: 85.5%, colorless powder).

Quelle