反应详情

Combine 2-((6-chloro-3-(4-chloro-2-fluorobenzoyl)-2-methylimidazo[1,2-b]pyridazin-8-yl)methyl)isoindoline-1,3-dione (7.30 g, 15.1 mmol), ethanol (200 mL), and hydrazine (1.45 mL, 3 equiv.) in a round bottom flask and place under nitrogen. Stir for 2 days at RT. Heat for 2 h at 50° C. then concentrate the reaction in vacuo. Dilute with EA. Wash the organics with 1 N HCl (aq) to pull product into the aqueous layer. Make the aqueous layer basic with 1 N NaOH (aq) and extract with EA. Wash the EA layer with aqueous saturated sodium chloride, and dry over anhydrous magnesium sulfate. Filter and concentrate in vacuo to give the title compound crude (1.2 g, 23%) as a light green solid. MS=355.0, 353.0 (M+1).

1. temperatureHeat for 2 h at 50° C.
2. concentrationthen concentrate
3. customthe reaction in vacuo
4. washWash the organics with 1 N HCl (aq)
5. extractionextract with EA
6. washWash the EA layer with aqueous saturated sodium chloride
7. dry with materialdry over anhydrous magnesium sulfate
8. filtrationFilter
9. concentrationconcentrate in vacuo