反应详情

To a mixed solution of the compound (1.3 g) obtained in Step 6, ammonium formate (1.2 g) and ethanol (13 ml) was added 10% palladium carbon (1.3 g) at 80° C. After stirring at the same temperature for 30 min, ammonium formate (1.3 g) and 10% palladium carbon (0.50 g) were added. After stirring at 80° C. for 30 min, ammonium formate (1.2 g) and 10% palladium carbon (0.65 g) were further added. After stirring at the same temperature for 1.5 hr, the reaction mixture was allowed to return to room temperature and diluted with chloroform. The mixture was filtered through celite, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:chloroform=1:2) to give the title compound (0.91 g).

1. stirringAfter stirring at 80° C. for 30 min
2. stirringAfter stirring at the same temperature for 1.5 hr
3. customto return to room temperature
4. filtrationThe mixture was filtered through celite
5. concentrationthe filtrate was concentrated under reduced pressure
6. customThe residue was purified by silica gel column chromatography (ethyl acetate:chloroform=1:2)