反应详情

A suspension of 1-(2,4-difluorophenoxy)-4-nitrobenzene (209 g, 1.17 mol) and 10% palladium-on-carbon (20 g, 50% wet) in methanol (1.0 L) was shaken under an atmosphere of hydrogen (60 psi) at room temperature for 5 h. The mixture was filtered through a plug of Celite® (150 g), washing with methanol (2×300 mL) and the solvent was removed under reduced pressure to afford the crude product as a dark red oil. This residue was triturated with hexanes (500 mL) and filtered to provide the title compound as a gray solid (175 g, 95%).1H NMR(300 MHz, DMSO-d6): 6.55(2H,d,J=8.8), 6.73(2H,d,J=8.8), 7.02-6.95(2H,m), 7.40(1H,t,J=11.4).

1. filtrationThe mixture was filtered through a plug of Celite® (150 g)
2. washwashing with methanol (2×300 mL)
3. customthe solvent was removed under reduced pressure
4. customto afford the crude product as a dark red oil
5. customThis residue was triturated with hexanes (500 mL)
6. filtrationfiltered