反应详情

温度

130 °C

6-Chloro-4-(5-methanesulfonyl-pyridin-2-ylamino)-2-methyl-2H-pyridazin-3-one (40 mg, 127 μmol, Eq: 1.00), 2-(6-tert-butyl-8-fluoro-1-oxophthalazin-2(1H)-yl)-6-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzyl acetate (136 mg, 165 μmol, Eq: 1.3) and cesium carbonate (145 mg, 445 μmol, Eq: 3.5) were dissolved in 10% aq. dioxane solution (3.3 ml). The reaction mixture was heated to 130° C. for 30 min in the microwave. Reaction mixture was filtered over celite. Filtrate was extracted with ethyl acetate, washed with water, and then with brine. Organic phase was dried over sodium sulfate; filtered; concentrated to give light brown solid. The crude material was dissolved in ethyl acetate, and treated with hexane until a precipitate was formed. Precipitate was collected by filtration to give an off-white solid. Solid was dissolved in dioxane (2 ml) and 1 M sodium hydroxide solution (191 μl, 191 μmol, Eq: 1.5) was added and stirred at room temperature overnight.+

1. customReaction mixture
2. filtrationwas filtered over celite
3. extractionFiltrate was extracted with ethyl acetate
4. washwashed with water
5. dry with materialOrganic phase was dried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customto give light brown solid
9. customwas formed
10. filtrationPrecipitate was collected by filtration
11. customto give an off-white solid