HRID2233076

反应详情

EQUATION

反应方程式

HRID 2233076 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 2-(4-fluorophenyl)imidazo[1,2-a]pyrazine (Preparation #2, 0.964 g, 4.52 mmol), 4-iodo-2-(methylthio)pyrimidine (Frontier, 2.28 g, 9.04 mmol), Cs2CO3 (2.21 g, 6.78 mmol), triphenylphosphine (0.474 g, 1.84 mmol), palladium acetate (0.203 g, 0.904 mmol), and DMF (10.5 mL) was heated at about 80° C. for about 13 h. The mixture was cooled to ambient temperature, diluted with water, and extracted with EtOAc. The combined organic layers were washed with brine, dried over MgSO4, filtered, and concentrated under reduced pressure. The resulting material was triturated with EtOAc and filtered to yield the title compound (0.640 g, 41%): LC/MS (Table 1, Method b) Rt=2.0 min; MS m/z: 338.4 (M+H)+.

WORKUP

后处理

  1. temperatureThe mixture was cooled to ambient temperature
  2. extractionextracted with EtOAc
  3. washThe combined organic layers were washed with brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe resulting material was triturated with EtOAc
  8. filtrationfiltered