反应详情

To a solution of 0.88 g of Compound [82], which had been obtained in Referential Example 12, dissolved in 25 ml of 80% aqueous formic acid, 1.8 g of Raney nickel were added, followed by heating under reflux for 1.5 hours. The reaction mixture was concentrated under reduced pressure. The residue so obtained was extracted with ethyl acetate. The extract was washed with aqueous sodium bicarbonate, dried over anhydrous magnesium sulfate and then filtered. The filtrate was concentrated under reduced pressure. The residue was purified by subjecting same to chromatography on a silica gel column using gradient elution with hexane-ethyl acetate, whereby 0.71 g of the title compound was obtained (yield: 80%).

1. temperatureby heating
2. temperatureunder reflux for 1.5 hours
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. customThe residue so obtained
5. extractionwas extracted with ethyl acetate
6. washThe extract was washed with aqueous sodium bicarbonate
7. dry with materialdried over anhydrous magnesium sulfate
8. filtrationfiltered
9. concentrationThe filtrate was concentrated under reduced pressure
10. customThe residue was purified
11. washelution with hexane-ethyl acetate