反应详情

To a solution of 1.49 g (5.94 mmol) of 3,5-di-t-butyl-4-hydroxybenzoic acid and 889 mg (7.73 mmol) of N-hydroxysuccinimide in 60 ml of methylene chloride was added 1.38 g (7.13 mmol) of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride under ice-cooling with stirring and the mixture was stirred at room temperature for 30 minutes. Further 1.00 g (5.94 mmol) of 4-(3-aminopropylthio)pyridine was added and the mixture was stirred at room temperature for 8 hours. The reaction mixture was washed with water and dried. The solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate) to obtain 650 mg of the desired compound (27.3%, colorless powder), mp: 203.0°-240.0° C.

1. temperaturecooling
2. stirringthe mixture was stirred at room temperature for 30 minutes
3. stirringthe mixture was stirred at room temperature for 8 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)