HRID1961703

反应详情

EQUATION

反应方程式

HRID 1961703 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

Sodium hydride (60% in mineral oil, 161 mg, 4.03 mmol) was added to a suspension of 4-chloroaniline (489 mg, 3.83 mmol) in dimethylsulfoxide (10 mL). The mixture was stirred at 130° C. for 5 minutes. 2-Chloro-6-(3,5-dimethyl-pyrazol-1-yl)-pyrazine was added and the resulting mixture was stirred at 130° C. for 30 minutes. Cooling, followed by addition of water gave a brown precipitate. The brown solid was collected by filtration, re-dissolved in ethyl acetate, washed with brine, dried over sodium sulphate, filtrated and evaporated. The crude product was purified by flash chromatography to give (4-chloro-phenyl)-[6-(3,5-dimethyl-pyrazol-1-yl)-pyrazin-2-yl]-amine (318 mg, 55%) as a brown solid.

WORKUP

后处理

  1. stirringthe resulting mixture was stirred at 130° C. for 30 minutes
  2. temperatureCooling
  3. customgave a brown precipitate
  4. filtrationThe brown solid was collected by filtration
  5. dissolutionre-dissolved in ethyl acetate
  6. washwashed with brine
  7. dry with materialdried over sodium sulphate
  8. filtrationfiltrated
  9. customevaporated
  10. customThe crude product was purified by flash chromatography