反应详情

4-{(3R,5S)-3-[(tert-Butoxycarbonyl)amino]-4-hydroxy-4,5-dimethylpiperidin-1-yl}-3-nitro-6,7-dihydro-5H-cyclopenta[b]pyridin-7-yl acetate (198 mg, 0.426 mmol) was dissolved in acetic acid (2.8 mL), and iron powder (0.36 g, 6.4 mmol) was added to the solution. Reaction was stirred at room temperature for 2 h. The mixture was diluted with 30 mL of EtOAc, filtered through diatomaceous earth. The filtrate was concentrated under reduced pressure and the resulting residue was dissolved in EtOAc, and neutralized with NaHCO3. The layers were separated, and the aqueous layer was extracted with further EtOAc. The combined organic layers were dried and concentrated under reduced pressure to give the sub-title compound as a white solid (176 mg, 95%), which was used in the next step without further purification. LCMS calc. for C22H35N4O5 (M+H)+ m/z=435.3. found 435.1.

1. customReaction
2. filtrationfiltered through diatomaceous earth
3. concentrationThe filtrate was concentrated under reduced pressure
4. dissolutionthe resulting residue was dissolved in EtOAc
5. customThe layers were separated
6. extractionthe aqueous layer was extracted with further EtOAc
7. customThe combined organic layers were dried
8. concentrationconcentrated under reduced pressure