반응 #6217

반응 방정식

4-(3-aminopropylthio)pyridine

thiophene-3-carboxylic acid

N-hydroxysuccinimide

1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride

→

desired compound

수율 76.1%

4-[3-(3-thiophenecarbonylamino)propylthio]pyridine

수율 76.1%

용매

methylene chloride

반응 조건

후처리

1. 1
   온도cooling
2. 2
   workup.STIRRINGThe mixture was stirred at room temperature for 1 hour
3. 3
   workup.STIRRINGthe mixture was stirred at room temperature for 2 hours
4. 4
   세척The reaction mixture was washed with water
5. 5
   기타dried
6. 6
   workup.DISTILLATIONthe solvent was distilled off
7. 7
   기타The residue was purified by column chromatography (eluent: methanol/ethyl acetate=1:10)

실험 절차

To a solution of 1.00 g (7.80 mmol) of thiophene-3-carboxylic acid and 1.08 g (10.1 mmol) of N-hydroxysuccinimide in 70 ml of methylene chloride, 1.80 g (9.36 mmol) of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride was added under ice-cooling with stirring. The mixture was stirred at room temperature for 1 hour. Further, 1.31 g (7.80 mmol) of 4-(3-aminopropylthio)pyridine was added, and the mixture was stirred at room temperature for 2 hours. The reaction mixture was washed with 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 1.65 g of the desired compound (yield: 76.1%, colorless powder).

출처