反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
2-Chloro-N-methyl-6-((2,2,2-trifluoroethoxy)methyl)pyrimidin-4-amine (161 mg, 0.63 mmol), 3-methoxy-4-(4-methyl-1H-imidazol-1-yl)aniline (256 mg, 1.26 mmol), cesium carbonate (410 mg, 1.26 mmol), palladium(II) acetate (21 mg, 0.09 mmol) and 2-(dicyclohexylphosphino)biphenyl (33 mg, 0.09 mmol) were mixed in dioxane (10 mL) under an atmosphere of nitrogen. The vial was heated in microwave reactor at 120° C. for 90 min. The mixture was filtered through a plug of diatomeous earth which was eluted with MeOH. The mixture was partitioned between EtOAc and sodium hydroxide (1 M, aq). The organic layer was dried over sodium sulfate and concentrated in vacuum. The residue was purified by preparative HPLC to give the title compound as a solid 136 mg (51%).
WORKUP
后处理
- filtrationThe mixture was filtered through a plug of diatomeous earth which
- washwas eluted with MeOH
- customThe mixture was partitioned between EtOAc and sodium hydroxide (1 M, aq)
- dry with materialThe organic layer was dried over sodium sulfate
- concentrationconcentrated in vacuum
- customThe residue was purified by preparative HPLC