反应详情

To a solution of 4-(3-chloro-4-(3-fluorobenzyloxy)phenylamino)-6-(1-oxo-2-butyn-1-yl)quinazoline (IV) (10 g) in 1,4-dioxane (300 mL) was added 2-(acetoxy)ethoxyamine (1.5 equiv) and then 2 mol/L methane sulfonic acid aq. solution (28 mL) and stirred for 17 hr at 60° C. The reaction mixture was poured into saturated sodium hydrogen carbonate aq. solution and extracted with ethyl acetate. Organic layer was washed with water and dried over sodium sulfate. The filtrate was concentrated and the residue was recrystallized from hydrous ethanol-water, filtered and dried to give 4-(3-chloro-4-(3-fluorobenzyloxy)phenylamino)-6-(1-(2-hydroxyethoxyimino)-2-butyn-1-yl)quinazoline (VIII) (7.6 g) as a colorless solid.

1. extractionextracted with ethyl acetate
2. washOrganic layer was washed with water
3. dry with materialdried over sodium sulfate
4. concentrationThe filtrate was concentrated
5. customthe residue was recrystallized from hydrous ethanol-water
6. filtrationfiltered
7. customdried