反应详情

温度

120 °C

8-Bromo-2,6-bis-((R)-3-methyl-morpholin-4-yl)-9-(tetrahydro-pyran-2-yl)-9H-purine (40 mg, 83 μmol) was dissolved in 2 mL of toluene under argon in a microwave vial, and 2-(tributylstannyl)-pyridine (36 mg, 83 μmol) and Pd(PPh3)4 (4.8 mg, 4.2 μmol) were added. The microwave vial was capped, and the reaction mixture was stirred for 3 hours at 120° C. The vial was cooled to room temperature and opened. The mixture was diluted with EtOAc (20 mL) and brine. The organic layer was separated, dried over Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by column chromatography (12 g SiO2, heptane/TBME in a gradient from 4/1 to 2/3) to give the product as a solid (35 mg, 88%).

1. additionwere added
2. customThe microwave vial was capped
3. temperatureThe vial was cooled to room temperature
4. customThe organic layer was separated
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe residue was purified by column chromatography (12 g SiO2, heptane/TBME in a gradient from 4/1 to 2/3)