反应详情

To a solution of 3-Chloro-5-fluoro-4-(quinolin-3-yloxy)nitrobenzene (186.1) (0.980 g) and NH4Cl (1.64 g) in EtOH (50 ml)-H2O (5 ml), was added iron powder (1.92 g). The mixture was heated to reflux for 1 hr. After cooling the reaction mixture was filtered through short celite pad. The filtrate was concentrated, diluted with sat. NaHCO3 and extacted with AcOEt (30 ml×3). The combined organic layeres were washed with brine and dried over Na2SO4. Concentration of solvent afford crude product, which was purified by column chromatography (silicagel, AcOEt:Hexane=1:3) to provide aniline 186.2 (0.420 g) as a colorless solid.

1. temperatureThe mixture was heated
2. temperatureto reflux for 1 hr
3. temperatureAfter cooling the reaction mixture
4. filtrationwas filtered through short celite pad
5. concentrationThe filtrate was concentrated
6. additiondiluted with sat. NaHCO3
7. washThe combined organic layeres were washed with brine
8. dry with materialdried over Na2SO4
9. customConcentration of solvent afford crude product, which
10. customwas purified by column chromatography (silicagel, AcOEt:Hexane=1:3)