HRID59139

反应详情

EQUATION

反应方程式

HRID 59139 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. filtrationThe mixture was filtered through a plug of diatomeous earth which
  2. washwas eluted with MeOH
  3. customThe mixture was partitioned between EtOAc and sodium hydroxide (1 M, aq)
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. concentrationconcentrated in vacuum
  6. customThe residue was purified by preparative HPLC