반응 #6218

반응 방정식

4-(3-aminopropylthio)pyridine

2-thienylacetic acid

N-hydroxysuccinimide

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

→

desired compound

수율 86.3%

4-[3-(2-thienylacetylamino)propylthio]pyridine

수율 86.3%

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)
8. 8
   기타to obtain powder
9. 9
   기타The powder thus obtained
10. 10
    세척was washed with ether
11. 11
    기타dried

실험 절차

To a solution of 913 mg (6.42 mmol) of 2-thienylacetic acid and 961 mg (8.35 mmol) of N-hydroxysuccinimide in 65 ml of methylene chloride, 1.48 g (7.70 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, 1.08 g (6.42 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 powder. The powder thus obtained was washed with ether and dried to obtain 1.62 g of the desired compound Lyield: 86.3%, pale yellow powder).

출처