HRID1528081

反应详情

EQUATION

反应方程式

HRID 1528081 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A suspension of 5-methoxy-3-(1-phenyl-1H-pyrazol-5-yl)pyridazin-4-ol (100 mg), 5-bromopyrimidine (119 mg), potassium carbonate (155 mg), copper(I) iodide (14 mg) and 4,7-dimethoxy-1,10-phenanthroline (20 mg) in DMSO (2 mL) was stirred at 110° C. for 40 hr under an argon atmosphere. To the reaction mixture was added aqueous sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by basic silica gel column chromatography (ethyl acetate/methanol), and recrystallized from ethyl acetate/hexane to give the title compound (11 mg).

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe extract was dried over anhydrous sodium sulfate
  3. customthe solvent was evaporated under reduced pressure
  4. customThe residue was purified by basic silica gel column chromatography (ethyl acetate/methanol)
  5. customrecrystallized from ethyl acetate/hexane