反应详情

温度

90 °C

A mixture of 4-(2,6-dichloro-5-methylsulfanyl-pyrimidin-4-yl)-morpholine (200 mg, 0.717 mmol.), 3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine (323 mg, 1.577 mmol, 2.2 eq), (PPh3)4Pd (165 mg, 0.2 mmol.), 2M Na2CO3 (2.1 ml, 4.302 mmol, 6.0 eq.) and dioxane (20 ml) was added to a reaction vessel which was then flushed with argon. The reaction mixture was stirred at 90° C. for 16 hrs, and then dried. The solvent was removed by evaporation. The mixture was partitioned between EA and water. The organic layer was collected, washed with brine, dried over MgSO4, filtered and evaporated in vacuo. The resulting residue was purified using flash chromatography on silica gel (Hexane/EtOAc 2:3, few Et3N), recrystallized by (Hexane/EtOAc) to give a pale yellow solid 57.8 mg (22.1%).

1. additionwas added to a reaction vessel which
2. customwas then flushed with argon
3. customdried
4. customThe solvent was removed by evaporation
5. customThe mixture was partitioned between EA and water
6. customThe organic layer was collected
7. washwashed with brine
8. dry with materialdried over MgSO4
9. filtrationfiltered
10. customevaporated in vacuo
11. customThe resulting residue was purified
12. customrecrystallized by (Hexane/EtOAc)