反应详情

To a solution of crude (2S,4R)-1-p-nitrobenzyloxycarbonyl -4-methanesulfonyloxy-2-pyrrolidinethiocarboxylic acid (4.0 g) obtained in Example 8 in methylene chloride (40 ml) was added pyridine (1.91 g). The mixture was heated under refluxing for 7 hours. After the reaction was over, the mixture was washed with aqueous 1 mole/1 hydrochloric acid solution. The organic layer was dried over magnesium sulfate. After the solvent was distilled, residue was purified by silica gel chromatography to give (1S,4S)-5-p-nitrobenzyloxycarbonyl-2-thia-5-azabicyclo-[2.2.1]heptan-3-one.

1. temperatureThe mixture was heated
2. temperatureunder refluxing for 7 hours
3. washwas washed with aqueous 1 mole/1 hydrochloric acid solution
4. dry with materialThe organic layer was dried over magnesium sulfate
5. distillationAfter the solvent was distilled
6. customresidue was purified by silica gel chromatography