HRID982636

反应详情

EQUATION

反应方程式

HRID 982636 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-(4-fluoro-phenyl)-3-(4-methanesulfonyl-phenyl)-pyrazolo[1,5-b]pyridazin-6-ol (0.2 g) in anhydrous dimethyl formamide (5 ml) was treated with sodium hydride ( 0.046 g, 60% dispersion in mineral oil), after effervescence ceased a stream of bromodifluoromethane gas was passed through the mixture at ambient temperature for 30 minutes. The reaction mixture was then poured into water (50 ml) and extracted with ethyl acetate (50 ml), the organic extract was washed with water (3×50 ml), dried and concentrated in vacuo. The residue was purified by chromatography to give the title compound as a white solid (0.17 g).

WORKUP

后处理

  1. extractionextracted with ethyl acetate (50 ml)
  2. extractionthe organic extract
  3. washwas washed with water (3×50 ml)
  4. customdried
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by chromatography