反应详情

To a mixture of 4′-amino-2′-fluoro-5′-nitrobiphenyl-4-carbonitrile (Preparation 90, 0.5 g, 2 mmol) and zinc dust (0.78 g, 12 mmol) in methanol (10 mL) was added ammonium chloride (0.41 g, 8 mmol) and the reaction was stirred at room temperature for 3 hours. The reaction was filtered through celite washing through with methanol (40 mL). The filtrate was concentrated to afford a solid that was purified using silica gel column chromatography eluting with EtOAc:heptanes 1:1 to afford the title compound as a brown solid (0.45 g, 99%).

1. filtrationThe reaction was filtered through celite
2. washwashing through with methanol (40 mL)
3. concentrationThe filtrate was concentrated
4. customto afford a solid
5. customthat was purified
6. washeluting with EtOAc:heptanes 1:1