反应详情

A solution of (3RS)-3-[(2S)-1-[3-(N-benzyl-N-methylcarbamoyl)propanoyl]pyrrolidin-2-yl]-3-hydroxy-2,2-difluoropropionic acid ethyl ester (250 mg) in methylene chloride (1.5 ml) was added dropwise to a suspension of Dess-Martin reagent (448 mg) in methylene chloride (6 ml). The mixture was stirred for 3 hrs. The reaction mixture was diluted with ether. A saturated aq. solution of sodium bicarbonate (30 ml) wherein sodium thiosulfate (2.26 g) was dissolved was added to the diluted solution. The mixture was stirred for 10 mins, and 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 (238 mg) having the following physical data:

1. additionwas added to the diluted solution
2. stirringThe mixture was stirred for 10 mins
3. extractionextracted with EtOAc
4. washThe extract was washed
5. customdried
6. customevaporated
7. customThe residue was purified by column chromatography on silica gel (hexane-EtoAc)