反应详情

Sodium carbonate (2.40 g, 22.7 mmol) and tetrakis triphenylphosphine palladium (0.44 g, 0.38 mmol) were added to a 1,4-dioxane (44.0 ml)-water (22.0 ml) mixture solution of 2-chloro-9-(cyclopropylmethyl)-6-morpholin-4-yl-9H-purine (2.22 g, 7.56 mmol) and 2-methylaminopyrimidine-5-boronic acid pinacol ester (2.31 g, 9.82 mmol) at room temperature and the resulting mixture was heated to reflux for 3.5 hours in an argon atmosphere. The reaction mixture was left standing to cool and then poured into water and ethyl acetate was added to separate the layers. The solid precipitated in the aqueous layer was collected by filtration, washed with water, and then dried at 50° C. under reduced pressure. Meanwhile, the organic layer was dried over anhydrous sodium sulfate, the mixture was filtrated, then the filtrate was concentrated under reduced pressure, and the resulting solid was washed with dichloromethane and collected by filtration. These solids were combined to give the title compound (1.68 g, 61%) as a white solid.

1. temperaturethe resulting mixture was heated
2. temperatureto reflux for 3.5 hours in an argon atmosphere
3. waitThe reaction mixture was left
4. temperatureto cool
5. additionwas added
6. customto separate the layers
7. customThe solid precipitated in the aqueous layer
8. filtrationwas collected by filtration
9. washwashed with water
10. customdried at 50° C. under reduced pressure
11. dry with materialMeanwhile, the organic layer was dried over anhydrous sodium sulfate
12. filtrationthe mixture was filtrated
13. concentrationthe filtrate was concentrated under reduced pressure
14. washthe resulting solid was washed with dichloromethane
15. filtrationcollected by filtration