反应详情

To a suspension of 4′-amino-2-fluoro-3′-nitrobiphenyl-4-carbonitrile (Preparation 92, 3 g, 11.66 mmol) in AcOH/THF (70 mL/70 mL) was added zinc dust (6.9 g, 105.6 mmol) and the reaction stirred at room temperature for 18 hours. The reaction was filtered and the filtrate concentrated in vacuo. The residue was treated with saturated aqueous NaHCO3 solution (200 mL) and extracted with EtOAc (200 mL). The organic layer was collected, dried over Na2SO4 and concentrated in vacuo. The solid was triturated with MTBE (30 mL) and filtered to afford the title compound as a brown solid (1.5 g, 57%).

1. filtrationThe reaction was filtered
2. concentrationthe filtrate concentrated in vacuo
3. additionThe residue was treated with saturated aqueous NaHCO3 solution (200 mL)
4. extractionextracted with EtOAc (200 mL)
5. customThe organic layer was collected
6. dry with materialdried over Na2SO4
7. concentrationconcentrated in vacuo
8. customThe solid was triturated with MTBE (30 mL)
9. filtrationfiltered