HRID466029

反应详情

EQUATION

反应方程式

HRID 466029 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of sodium methoxide in methanol (28%, 411 mg) was added to a mixture of 3-(3-chloropyridazin-6-yl)-2-phenylpyrazolo[1,5-a]pyridine (436 mg) and methanol (4 ml) at room temperature. The reaction mixture was heated under reflux for 3 hours. After evaporating the solvent in vacuo, a saturated aqueous solution of sodium chloride (20 ml) was added to the residue and extracted with chloroform (20 ml×3). The combined extract was washed with a saturated aqueous solution of sodium chloride (20 ml), dried over magnesium sulfate and evaporated in vacuo. The residue was purified by column chromatography on silica gel (10 g) using chloroform as an eluent and recrystallized from 95% EtOH to give 3-(3-methoxypyridazin-6-yl)-2-phenylpyrazolo[1,5-a]pyridine (165 mg).

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureunder reflux for 3 hours
  3. customAfter evaporating the solvent in vacuo
  4. additiona saturated aqueous solution of sodium chloride (20 ml) was added to the residue
  5. extractionextracted with chloroform (20 ml×3)
  6. extractionThe combined extract
  7. washwas washed with a saturated aqueous solution of sodium chloride (20 ml)
  8. dry with materialdried over magnesium sulfate
  9. customevaporated in vacuo
  10. customThe residue was purified by column chromatography on silica gel (10 g)
  11. customrecrystallized from 95% EtOH