HRID59133

反应详情

EQUATION

反应方程式

HRID 59133 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

A mixture of 2-chloro-N-methyl-6-((2,2,2-trifluoroethoxy)methyl)pyrimidin-4-amine (85 mg, 0.33 mmol), 4-(4-methyl-1H-imidazol-1-yl)aniline (100 mg, 0.58 mmol), cesium carbonate (217 mg, 0.67 mmol), palladium(II) acetate (11 mg, 0.05 mmol) and 2-(dicyclohexylphosphino)-biphenyl (17 mg, 0.05 mmol) in dioxane (3 mL) was heated in a microwave reactor under notrogen atmosphere at 120° C. for 90 min. The reaction mixture was filtered through a pad of diatomeous earth which was eluted with MeOH. The mixture was partitioned between EtOAc and sodium hydroxide (aq, 1 M). The organic phase was separated, dried over sodium sulfate and concentrated in vacuum. The residue was purified by preparative HPLC to give the title compound as a solid 52 mg, (40%).

WORKUP

后处理

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