反应详情

5-(2-Butoxy-5-iodo-3-pyridinyl)-3-ethyl-2-(2-methoxyethyl)-2,6-dihydro-7H-pyrazolo[4,3-d]pyrimidin-7-one (Example 1) (140 mg, 0.28 mmol), K2CO3 (78 mg, 0.56 mmol) and 3-trifluoromethylboronic acid (60 mg, 0.34 mmol) were stirred together in aqueous dioxan under a nitrogen atmosphere. The mixture was immersed in a pre-heated oil bath at 120° C. for a few minutes and Pd(PPh3)4 (34 mg, 0.028 mmol) was added. The mixture was heated at reflux for 2 h and then cooled. The cooled mixture was concentrated and partitioned between ethyl acetate and water. This was then filtered through an Arbocel® pad to remove the palladium residues and the organic layer separated, washed with sodium bicarbonate solution then brine, dried (MgSO4) and concentrated. Recrystallisation from ethyl acetate gave the title compound (101 mg, 70%).

1. waitThe mixture was immersed in a pre-heated oil bath at 120° C. for a few minutes
2. temperatureThe mixture was heated
3. temperatureat reflux for 2 h
4. temperaturecooled
5. concentrationThe cooled mixture was concentrated
6. custompartitioned between ethyl acetate and water
7. filtrationThis was then filtered through an Arbocel® pad
8. customto remove the palladium residues
9. customthe organic layer separated
10. washwashed with sodium bicarbonate solution
11. dry with materialbrine, dried (MgSO4)
12. concentrationconcentrated
13. customRecrystallisation from ethyl acetate