反应详情

温度

65 °C

To a solution of ethyl 6-fluoro-4-hydroxypyrrolo[1,2-b]pyridazine-3-carboxylate (700 mg, 3.12 mmol) in methanol (3 mL) and THF (3 mL) was added 3 N aq. sodium hydroxide (5.20 mL, 15.61 mmol) and the resulting mixture was stirred at 65° C. for 3 h. The mixture was cooled and concentrated to remove the methanol and THF and the obtained residue was cooled in an ice bath and 3N aq. HCl was added dropwise with stirring until pH of the mixture was ˜2. The resulting slurry was stirred for 30 min, and filtered to collect the solid. The solid was rinsed with water and dried to afford 550 mg (90%) of the title compound as a white solid. HPLC (condition B): retention time=2.37 min. LCMS (condition B): m/z 197+ve.

1. temperatureThe mixture was cooled
2. concentrationconcentrated
3. customto remove the methanol and THF
4. temperaturethe obtained residue was cooled in an ice bath
5. addition3N aq. HCl was added dropwise
6. stirringwith stirring until pH of the mixture
7. stirringThe resulting slurry was stirred for 30 min
8. filtrationfiltered
9. customto collect the solid
10. washThe solid was rinsed with water
11. customdried