反应详情

To a solution of 3-chloro-5-fluorophenyl 4-nitrophenyl ether (Intermediate 5, 2.38 g) in THF (40 mL) and water (10 mL) was added Fe power (11.2 g, 200 mmol) and ammonium chloride (10.7 g, 200 mmol). The reaction mixture was heated at reflux for 4 hours. After filtration, the solvent was concentrated to give a residue and poured into 50 mL of water. The mixture was extracted with ethyl acetate (3 times 50 mL) and the combined organic phases were washed and dried over magnesium sulphate. Removal of the solvent afforded the title compound (2.02 g) which was directly used in the next step.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 4 hours
3. filtrationAfter filtration
4. concentrationthe solvent was concentrated
5. customto give a residue
6. extractionThe mixture was extracted with ethyl acetate (3 times 50 mL)
7. washthe combined organic phases were washed
8. dry with materialdried over magnesium sulphate
9. customRemoval of the solvent