反应详情

To a solution (20 mL) of methyl 4-{[(5-bromo-3-methylfuro[3,2-b]pyridin-2-yl)(cyclohexyl)methyl]amino}benzoate (1.86 g) synthesized above in tetrahydrofuran was added 2N lithium hydroxide aqueous solution (10.2 mL), and the mixture was stirred with heating under reflux for 2 hr. A 4N aqueous lithium hydroxide solution (5.10 mL) was additionally added, and the mixture was stirred with heating under reflux for 4 hr. A 4N aqueous lithium hydroxide solution (5.10 mL) and ethanol (20 mL) were further added, and the mixture was stirred with heating under reflux for 4 hr, and concentrated under reduced pressure. The residue was dissolved in water (40 mL), and 1N hydrochloric acid (61.2 mL) was added at 0° C. The resulting precipitate was collected by filtration to give the title object compound (1.74 g, 96%) as a pale-brown solid.

1. temperaturewith heating
2. temperatureunder reflux for 2 hr
3. stirringthe mixture was stirred
4. temperaturewith heating
5. temperatureunder reflux for 4 hr
6. stirringthe mixture was stirred
7. temperaturewith heating
8. temperatureunder reflux for 4 hr
9. concentrationconcentrated under reduced pressure
10. dissolutionThe residue was dissolved in water (40 mL)
11. addition1N hydrochloric acid (61.2 mL) was added at 0° C
12. filtrationThe resulting precipitate was collected by filtration