反应详情

To a solution of 2.55 g (8.91 mmol) of 4,5-dibromothiophene-2-carboxylic acid and 1.33 g (11.6 mmol) of N-hydroxysuccinimide in 90 ml of methylene chloride, 2.05 g (10.7 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, 1.50 g (8.91 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: ethyl acetate) to obtain powder. The powder thus obtained was washed with ether and dried to obtain 2.79 g of the desired compound (yield: 71.8%, colorless powder).

1. temperaturecooling
2. stirringThe mixture was stirred at room temperature for 1 hour
3. stirringthe mixture was stirred at room temperature for 2 hours
4. washThe reaction mixture was washed with water
5. customdried
6. distillationthe solvent was distilled off
7. customThe residue was purified by column chromatography (eluent: ethyl acetate)
8. customto obtain powder
9. customThe powder thus obtained
10. washwas washed with ether
11. customdried