反应详情

To a mixture of nitro compound 379 (279 mg, 0.72 mmol) and NH4Cl (33 mg, 0.612 mmol) in EtOH (7.2 mL)/water (3.6 mL) at 100° C. Fe powder (342 mg, 6.2 mmol) was added in one portion and the mixture was heated to reflux with vigorous stirring for 40 min. The mixture was filtered through Celite®, the Celite® washed with EtOH and the combined filtrates were concentrated under reduced pressure. The residue was dissolved in MeOH and purified by flash chromatography (DCM/MeOH 5:1) providing 376 (171.3 mg, 0.48 mmol, 67% yield) as a yellow solid. LCMS:(M+H) 356.0.

1. temperaturethe mixture was heated
2. temperatureto reflux
3. filtrationThe mixture was filtered through Celite®
4. washthe Celite® washed with EtOH
5. concentrationthe combined filtrates were concentrated under reduced pressure
6. dissolutionThe residue was dissolved in MeOH
7. custompurified by flash chromatography (DCM/MeOH 5:1)