反应详情

A dioxane (5 ml)-water (1 ml) suspension of 2-chloro-9-isobutyl-6-[(3S)-3-methylmorpholin-4-yl]-9H-purine (317 mg, 1.02 mmol), 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyrimidin-2-amine (226 mg, 1.02 mmol), sodium carbonate (325 mg, 3.07 mmol), and tetrakis triphenylphosphine palladium (118 mg, 0.10 mmol) was heated to reflux for 2.5 hours. The reaction mixture was returned to room temperature. Water was added to the reaction mixture and the resulting mixture was extracted with chloroform. The organic layer was dried over anhydrous magnesium sulfate and, after filtration, the filtrate was concentrated under reduced pressure. The residue was purified by flash silica gel column chromatography (methylene chloride:methanol=96:4). The residue was purified by flash silica gel column chromatography (ethyl acetate) to give the title compound (287 mg, 76%) as a solid.

1. temperaturewas heated
2. temperatureto reflux for 2.5 hours
3. customwas returned to room temperature
4. extractionthe resulting mixture was extracted with chloroform
5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
6. filtrationafter filtration
7. concentrationthe filtrate was concentrated under reduced pressure
8. customThe residue was purified by flash silica gel column chromatography (methylene chloride:methanol=96:4)
9. customThe residue was purified by flash silica gel column chromatography (ethyl acetate)