反应详情

2-Cyano-4-nitrobiphenyl (0.067 moles, 15.0 g.) was dissolved in 100 ml ethyl acetate/100 ml ethanol and hydrogenated at 40 psi over 3.0 g of 10% palladium on carbon. The catalyst was removed by filtering though celite. The solvents were removed in vacuo. The residue was dissolved in 175 ml of methylene chloride. Acetic anhydride (15 ml) was added. The reaction was stirred at room temperature for 30 minutes and poured over ice. The organic layer was dried, concentrated, and then purified by HPLC over silica gel eluted with a gradient of 0-10% ethyl acetate in chloroform. (MS)

1. customThe catalyst was removed
2. filtrationby filtering though celite
3. customThe solvents were removed in vacuo
4. dissolutionThe residue was dissolved in 175 ml of methylene chloride
5. additionAcetic anhydride (15 ml) was added
6. additionpoured over ice
7. customThe organic layer was dried
8. concentrationconcentrated
9. custompurified by HPLC over silica gel
10. washeluted with a gradient of 0-10% ethyl acetate in chloroform