反应详情

To a mixed solution of the compound (66 mg) obtained in Step 5, ammonium formate (28 mg) and ethanol (1.3 ml) was added 10% palladium carbon (33 mg) with heating under reflux. The mixture was stirred at the same temperature for 10 min and ammonium formate (28 mg) and 10% palladium carbon (33 mg) were added and the mixture was stirred for 10 min. Ammonium formate (28 mg) and 10% palladium carbon (33 mg) were further added. The reaction mixture was allowed to return to room temperature, and diluted with ethanol. The mixture was filtered through celite, and the filtrate was concentrated under reduced pressure. The residue was partitioned by adding ethyl acetate and water. The organic layer was dried over anhydrous magnesium sulfate, filtrated, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform:methanol=20:1), and the obtained crude product was suspended in hexane, collected by filtration, and dried to give the title compound (31 mg).

1. temperaturewith heating
2. temperatureunder reflux
3. stirringthe mixture was stirred for 10 min
4. customto return to room temperature
5. filtrationThe mixture was filtered through celite
6. concentrationthe filtrate was concentrated under reduced pressure
7. customThe residue was partitioned
8. additionby adding ethyl acetate and water
9. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
10. filtrationfiltrated
11. concentrationconcentrated under reduced pressure
12. customThe residue was purified by silica gel column chromatography (chloroform:methanol=20:1)
13. customthe obtained crude product
14. filtrationcollected by filtration
15. customdried