反应详情

In a dry 50 mL round bottom flask 5-nitro-pyrimidin-2-ylamine (0.2 g, 1.36 mmol), intermediate 21 (Example 29) (0.61 g, 2.04 mmol), cesium carbonate (1.33 g, 4.08 mmol), 4,5-bis(diphenylphosphino)-9,9-dimethyl xanthene (0.157 g, 0.272 mmol) and tris(dibenzylideneacetone) dipalladium (0.124 g, 0.136 mmol) were combined. Reactants were flushed with argon, diluted with dioxane (8 mL) and outfitted with reflux condenser. Reaction was heated to reflux for 18 h. Reaction was then filtered hot and solvents were evaporated to provide dark solids. Silica gel chromatography (6:1 DCM/MeOH) provided desired product as a yellow powder (0.17 g, 33% yield). Rf=0.23 (10% MeOH/DCM)

1. customReactants were flushed with argon
2. additiondiluted with dioxane (8 mL)
3. temperaturewith reflux condenser
4. customReaction
5. temperaturewas heated
6. temperatureto reflux for 18 h
7. customReaction
8. filtrationwas then filtered hot
9. customsolvents were evaporated
10. customto provide dark solids