HRID457877

反应详情

EQUATION

反应方程式

HRID 457877 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of 4-(3-fluorophenyl)-5-(2-fluoro-4-pyridyl)-2-pyrimidinylamine (100 mg, 0.352 mmol) and ammonia/ethanol (ethanol saturated with an ammonia gas under ice-cooling) (20 mL) was sealed in a test tube and stirred at 150° C. for 2 weeks. After cooling as it was, the reaction solution was concentrated. The residue was dissolved by adding ethyl acetate and water thereto. The organic layer was washed with water and brine, and then dried over anhydrous sodium sulfate and concentrated. The residue was purified by TLC plate (eluting solvent: dichloromethane/methanol=10/1), to give the title compound (12 mg, 12%).

WORKUP

后处理

  1. temperaturecooling) (20 mL)
  2. customwas sealed in a test tube
  3. temperatureAfter cooling as it
  4. concentrationthe reaction solution was concentrated
  5. dissolutionThe residue was dissolved
  6. additionby adding ethyl acetate and water
  7. washThe organic layer was washed with water and brine
  8. dry with materialdried over anhydrous sodium sulfate
  9. concentrationconcentrated
  10. customThe residue was purified by TLC plate (eluting solvent: dichloromethane/methanol=10/1)