反应详情

Ethyl 3-amino-4-(aminocyclohexyl)benzoate (3.67 g, 13.99 mmol) was dissolved in DMF (10 mL) and water (1 mL). Oxone® (9.8 mmol, 6.02 g) was added followed by 3-furaldehyde (1.44 g, 15 mmol). The mixture was stirred 45 min at room temperature. 4 N NaOH (20 mL) was added and the mixture stirred at 60° C. for 18 h. After cooling to room temperature, water (100 mL) was added and insoluble impurities removed by filtration through celite. AcOH was then added to precipitate the product as a beige solid. The precipitated carboxylic acid was collected by filtration, washed with water and dried to give the title compound as a beige solid (3.69 g, 85% yield).

1. stirringthe mixture stirred at 60° C. for 18 h
2. temperatureAfter cooling to room temperature
3. custominsoluble impurities removed by filtration through celite
4. additionAcOH was then added
5. customto precipitate the product as a beige solid
6. filtrationThe precipitated carboxylic acid was collected by filtration
7. washwashed with water
8. customdried