HRID747167

反应详情

EQUATION

反应方程式

HRID 747167 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

In a reaction vessel, sodium hydride (15 mg, 0.372 mmol) was suspended in N,N-dimethylformamide (4 ml) and ethylene glycol (23 mg, 0.372 mmol) was added thereto, followed by stirring at 80° C. for 30 minutes under an atmosphere of nitrogen gas. Subsequently, 5-(2-fluoro-4-pyridyl)-4,6-di(2-furyl)-2-pyrimidinamine (100 mg, 0.310 mmol) was added thereto, followed by stirring for 14 hours under the same conditions. Then, the reaction was terminated by adding water thereto. The reaction mixture was extracted with ethyl acetate, washed with water and brine, dried over anhydrous sodium sulfate and then the filtrate was concentrated. The resulting crude product was purified by silica gel column chromatography, to give the title compound (41 mg, 36%) as a pale yellow solid.

WORKUP

后处理

  1. stirringby stirring for 14 hours under the same conditions
  2. customThen, the reaction was terminated
  3. additionby adding water
  4. extractionThe reaction mixture was extracted with ethyl acetate
  5. washwashed with water and brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationthe filtrate was concentrated
  8. customThe resulting crude product was purified by silica gel column chromatography