反应详情

Zinc powder (482 mg) and a small amount of iodine were added to a solution of ethyl bromoacetate (0.70 ml) in THF (6 ml). The mixture was refluxed for 30 mins. The solution was added dropwise to a solution of (2S)-1-[3-(N-benzyl-N-methylcarbamoyl)propanoyl)pyrrolidin-2-al (1.21 g) in benzene (10 ml). The mixture was refluxed for 30 mins. After reaction, 1N hydrochloric acid was added to the mixture. The mixture was extracted with EtOAc. The extract was washed, dried, and evaporated. The residue was purified by column chromatography on silica gel (hexane-EtOAc) to give the title compound (1.21 g) having the following physical data:

1. temperatureThe mixture was refluxed for 30 mins
2. temperatureThe mixture was refluxed for 30 mins
3. additionwas added to the mixture
4. extractionThe mixture was extracted with EtOAc
5. washThe extract was washed
6. customdried
7. customevaporated
8. customThe residue was purified by column chromatography on silica gel (hexane-EtOAc)