反应详情

温度

80 °C

To a solution of methyl 3-(imidazo[1,2-b]pyridazin-6-yloxy)benzoate (1665 mg, 6.18 mmol) in methanol (30 mL) was added 8N aqueous sodium hydroxide solution (3.00 mL), and the mixture was stirred at room temperature for 18 hr and at 80° C. for 8 hr. After the reaction mixture was allowed to cool to room temperature, 6N hydrochloric acid (4.00 mL) was added to the mixture, and the mixture was concentrated under reduced pressure. Water (30 mL) was added to the residue, and the precipitate was collected by filtration and washed with water. The precipitate was suspended in methanol (10 mL) and the suspension was stirred with heating under reflux for 10 min. After the suspension was allowed to cool to room temperature, the precipitate was collected by filtration washed with methanol and dried under reduced pressure to give the title compound (1045 mg, 4.09 mmol, yield 66%) as a white solid.

1. temperatureto cool to room temperature
2. concentrationthe mixture was concentrated under reduced pressure
3. additionWater (30 mL) was added to the residue
4. filtrationthe precipitate was collected by filtration
5. washwashed with water
6. stirringthe suspension was stirred
7. temperaturewith heating
8. temperatureunder reflux for 10 min
9. temperatureto cool to room temperature
10. filtrationthe precipitate was collected by filtration
11. washwashed with methanol
12. customdried under reduced pressure