反应详情

温度

0 °C

To a stirred solution of triphosgene (0.084 g, 0.28 mmol) in dichloromethane (1 ml) at 0° C. was slowly added a solution of 2-benzenesulfonylphenylamine (0.2 g, 0.87 mmol) in dichloromethane (1 ml) and the mixture was stirred at 0° C. for 15 minutes. After that, triethylamine (0.17 g, 1.74 mmol) in dichloromethane (2 ml) was added dropwise at 0° C. and the reaction was allowed to stir at room temperature for 3 h. To this solution a mixture of (S)-2-amino-3-[4-(2,6-dichlorobenzoylamino)phenyl]propionic acid methyl ester hydrochloride (0.35 g, 0.87 mmol) and triethylamine (0.9 g, 0.87 mmol) in dichloromethane (2 ml) was slowly added and the resulting reaction mixture was stirred at room temperature overnight. The volatiles were removed under reduced pressure and the residue was purified by column chromatography (Flash Biotage, dichloromethane:ethyl acetate 3:1) to yield the title compound (0.26 g, 50%) as a white solid.

1. stirringto stir at room temperature for 3 h
2. additionwas slowly added
3. customthe resulting reaction mixture
4. stirringwas stirred at room temperature overnight
5. customThe volatiles were removed under reduced pressure
6. customthe residue was purified by column chromatography (Flash Biotage, dichloromethane:ethyl acetate 3:1)