反应详情

Subsequently, to a suspension of iron (110 g) in acetic acid (500 ml) was added dropwise a solution of the obtained diethyl methyl(5-methyl-4-{[(3R)-1-{[(2-methyl-2-propanyl)oxy]carbonyl}-3-piperidinyl](2-propanyl)carbamoyl}-2-nitrophenoxy)propanedioate (205 g) in acetic acid (200 ml) slowly at 90° C. Ten hours later, the mixture was allowed to cool to room temperature, filtered through celite, and the filtrate was concentrated under reduced pressure. To the obtained residue was added a saturated aqueous sodium hydrogen carbonate solution, and the mixture was extracted with chloroform. The organic layer was washed with water and a saturated aqueous sodium chloride solution, dried over sodium sulfate, and filtered. The filtrate was concentrated under reduced pressure, and the resulting residue was purified by silica gel chromatography to give the title compound (102 g).

1. customTen hours
2. filtrationfiltered through celite
3. concentrationthe filtrate was concentrated under reduced pressure
4. additionTo the obtained residue was added a saturated aqueous sodium hydrogen carbonate solution
5. extractionthe mixture was extracted with chloroform
6. washThe organic layer was washed with water
7. dry with materiala saturated aqueous sodium chloride solution, dried over sodium sulfate
8. filtrationfiltered
9. concentrationThe filtrate was concentrated under reduced pressure
10. customthe resulting residue was purified by silica gel chromatography