反应详情

To a solution of 4.5 g of the compound obtained in Example 5 in 8.6 ml of pyridine was added 4.36 g of p-toluenesulfonyl chloride and the mixture was stirred under cooling with ice for 4 hours, and then at room temperature for 4 hours. To the mixture were added ethyl acetate and 1 N hydrochloric acid. The mixture was shaken, and the organic layer was separated. The organic layer was washed with water and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure. The residue was purified through silica gel column chromatography to yield 6.52 g of the titled compound.

1. temperatureunder cooling with ice for 4 hours
2. stirringThe mixture was shaken
3. customthe organic layer was separated
4. washThe organic layer was washed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. customThe solvent was removed under reduced pressure
7. customThe residue was purified through silica gel column chromatography