Reaktion #6233

Reaktionsgleichung

4-[3-(N-2-pyridylmethylamino)propylthio)pyridine

triethylamine

benzoyl chloride

→

desired compound

Ausbeute 58.9%

4-[3-(N-2-pyridylmethyl-N-benzoylamino)propylthio]pyridine

Ausbeute 58.9%

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/methanol=10:1)

Vorschrift

To a solution of 1.60 g (6.17 mmol) of 4-[3-(N-2-pyridylmethylamino)propylthio)pyridine and 1.05 ml (7.40 mmol) of triethylamine in 10 ml of methylene chloride, 0.86 ml (7.40 mmol) of benzoyl 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/methanol=10:1) to obtain 1.32 g of the desired compound (yield: 58.9%, yellow oil).

Quelle