반응 #6214

반응 방정식

3-(3-aminopropylthio)pyridine dihydrochloride

triethylamine

2-thenoyl chloride

→

desired compound

수율 85.4%

3-[3-(thenoylamino)propylthio]pyridine

수율 85.4%

용매

methylene chloride

반응 조건

후처리

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

실험 절차

To a solution of 2.00 g (8.29 mmol) of 3-(3-aminopropylthio)pyridine dihydrochloride and 4.16 ml (29.9 mmol) of triethylamine in 80 ml of methylene chloride, 1.06 ml (9.95 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 1.97 g of the desired compound (yield: 85.3%, yellow powder).

출처