反应详情

A solution of 5-nitroquinoline (50 g, 0.29 mol) in 1 L acetic acid and 30 mL acetic anhydride was treated with 5% Pd/C (3 g) and shaken on a Parr apparatus under a H2 atmosphere (50.8 psi) for 10.4 hours. The reaction was then treated with PtO2 (1 g) and recharged with H2 (50.8 psi) and shaken an additional 2 hours. After removing the catalyst by filtration, the filtrate was evaporated and the residue was separated between methylene chloride and water. The aqueous layer was basified with 50% NaOH and washed with methylene chloride. The combined organic layer was dried over sodium sulfate, filtered, and evaporated. The resulting solid was crystallized from ethyl acetate (23 g, 42%).

1. stirringshaken an additional 2 hours
2. customAfter removing the catalyst
3. filtrationby filtration
4. customthe filtrate was evaporated
5. customthe residue was separated between methylene chloride and water
6. washwashed with methylene chloride
7. dry with materialThe combined organic layer was dried over sodium sulfate
8. filtrationfiltered
9. customevaporated
10. customThe resulting solid was crystallized from ethyl acetate (23 g, 42%)