反应详情

Combine 4-(5-cyano-pyridin-2-yloxy)-benzamide (202 mg, 0.844 mmol), 5% Pd/C (80 mg) and conc. HCl (0.423 mL) in THF (4 mL) and EtOH (4 mL). Run the reaction under hydrogen atmosphere (1 atm) at rt overnight. Add NaOH (5 N, 2 mL) and filter the reaction mixture through Celite®. Concentrate the filtrate. Wash the residue with H2O (5 mL) and extract with CH2Cl2 (3× 5 mL). Combine the organic layers and purify through an SCX column eluting with 2M ammonia in methanol. Concentrate the fractions to give the title compound (74 mg, 36%).

1. customthe reaction under hydrogen atmosphere (1 atm) at rt overnight
2. filtrationAdd NaOH (5 N, 2 mL) and filter the reaction mixture through Celite®
3. concentrationConcentrate the filtrate
4. washWash the residue with H2O (5 mL)
5. extractionextract with CH2Cl2 (3× 5 mL)
6. customCombine the organic layers and purify through an SCX column
7. washeluting with 2M ammonia in methanol
8. concentrationConcentrate the fractions