反应详情

Under nitrogen atmosphere, 0.24 ml of trifluoromethansulfonic anhydride was added at 0° C. to 4 ml of pyridine solution with 180 g of 7-hydroxy-4H-chromen-4-one, and the mixture was stirred at room temperature for 5 hours. Water was added to the reaction solution, extracted with chloroform. Chloroform layer was washed with saturated saline solution, and then dried with anhydrous sodium sulfate. After distilling out the solvents under reduced pressure, residues were separated and purified with preparative thin-layer chromatography (chloroform/methanol=10/1) to obtain 83 mg of the above compound as a white solid.

1. extractionextracted with chloroform
2. washChloroform layer was washed with saturated saline solution
3. dry with materialdried with anhydrous sodium sulfate
4. distillationAfter distilling out the solvents under reduced pressure, residues
5. customwere separated
6. custompurified with preparative thin-layer chromatography (chloroform/methanol=10/1)