反应详情

温度

100 °C

Following Example 112a, 2-methoxypyrimidin-4-amine (0.625 g, 5 mmol), 3,5-dibromo-1-methyl-1H-pyridin-2-one (1.34 g, 5 mmol), cesium carbonate (4.88 g, 15 mmol), tris(dibenzylideneacetone)-dipalladium(0) (0.465 g, 0.5 mmol), Xantphos (0.58 g, 1 mmol) and 1,4-dioxane (50 mL) were heated at 100° C. for 24 hours. The mixture was cooled to room temperature, and filtered through a pad of Celite 521. The filter cake was washed with 9:1 methylene chloride/methanol (2×25 mL), and the combined filtrates were concentrated to dryness. The residue was dissolve in methylene chloride, diethyl ethyl was added, and the resulting precipitate was filtered to give a quantitative yield (1.57 g) of 263a as a green solid: MS (ESI+) m/z 313.1 (M+H).

1. temperatureThe mixture was cooled to room temperature
2. filtrationfiltered through a pad of Celite 521
3. washThe filter cake was washed with 9:1 methylene chloride/methanol (2×25 mL)
4. concentrationthe combined filtrates were concentrated to dryness
5. dissolutionThe residue was dissolve in methylene chloride
6. additiondiethyl ethyl was added
7. filtrationthe resulting precipitate was filtered