反应详情

A mixture of 1-(5-bromo-2-hydroxy-3-nitrophenyl)ethanone (25 g, 96 mmol), iron (27 g, 481 mmol), and NH4Cl (5.1 g, 96 mmol) in EtOH/H2O (5:1, 300 ml) was heated at reflux in 2 h, the mixture was cooled filtered the solid, the filtrate was concentrated, taken up in H2O, extracted with DCM (3×), dried over MgSO4, concentrated and purified by ISCO (10% EtOAc/Hexanes) to give the title compound as a yellow solid. MS (m+2): 232.1.

1. temperaturewas heated
2. temperatureat reflux in 2 h
3. temperaturethe mixture was cooled
4. filtrationfiltered the solid
5. concentrationthe filtrate was concentrated
6. extractionextracted with DCM (3×)
7. dry with materialdried over MgSO4
8. concentrationconcentrated
9. custompurified by ISCO (10% EtOAc/Hexanes)