反应详情

To a solution of 2-chloro-5-methylpyrimidin-4-amine (144 mg, 1.0 mmol) in 1,4-dioxane (20 mL) was added 4-bromo-2-chlorobenzonitrile (217 mg, 1.0 mmol), Cs2CO3 (1.3 g, 4.0 mmol), Pd2(dba)3 (91 mg, 0.1 mmol), and 4,5-bis(diphenylphosphino)-9,9-dimethyxanthene (Xant Phos, 173 mg, 0.3 mmol). The mixture was heated under reflux for 4 h under Ar. The solid was filtered off and the filtrate washed with brine (1×100 mL). The organic solution was separated and dried (Na2SO4). The solvent was removed until 5 mL and hexane (100 mL) was added, the solid was collected by filtration. The crude product, the title intermediate 26, was used for next reaction without further purification.

1. temperatureThe mixture was heated
2. temperatureunder reflux for 4 h under Ar
3. filtrationThe solid was filtered off
4. washthe filtrate washed with brine (1×100 mL)
5. customThe organic solution was separated
6. dry with materialdried (Na2SO4)
7. customThe solvent was removed until 5 mL and hexane (100 mL)
8. additionwas added
9. filtrationthe solid was collected by filtration
10. customThe crude product, the title intermediate 26, was used for next reaction without further purification