反应详情

To a mixture of the nitro compound 390 (358.2 mg, 0.87 mmol) and NH4Cl (39.4 mg, 0.74 mmol) in EtOH (8.7 mL)/water (4.3 mL) at 100° C. Fe powder (411.3 mg, 7.36 mmol) was added in one portion and the mixture was heated to reflux under vigorous stirring for 40 min. It was then filtered through Celite®, the Celite® was washed with EtOH and the combined filtrates were concentrated under reduced pressure. The residue was dissolved in DCM, washed with water, dried (anhydrous Na2SO4) and concentrated under reduced pressure affording 391 (256.5 mg, 77% yield) as a white solid. LCMS:(M+H) 384.2.

1. temperaturethe mixture was heated
2. temperatureto reflux
3. filtrationIt was then filtered through Celite®
4. washthe Celite® was washed with EtOH
5. concentrationthe combined filtrates were concentrated under reduced pressure
6. dissolutionThe residue was dissolved in DCM
7. washwashed with water
8. dry with materialdried (anhydrous Na2SO4)
9. concentrationconcentrated under reduced pressure