HRID498068

反应详情

EQUATION

反应方程式

HRID 498068 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-chloro-1-(2-pyridinyl)-1H-pyrazolo[3,4-b]quinoline (14 g, 0.050 mol) in ethanol (600 mL), 6N hydrochloric acid (30 mL) was added and the mixture was heated under reflux for 12 hours. The reaction solution was allowed to cool to room temperature, and concentrated and evaporated under reduced pressure. The residue was made basic by addition of an aqueous sodium hydroxide solution, and the organic matter was extracted with chloroform. The extract was washed with saturated brine and water, dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue thus obtained was purified by silica gel column chromatography (chloroform:methanol=96:4) to give the title compound (10.8 g, 82% yield).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 12 hours
  3. concentrationconcentrated
  4. customevaporated under reduced pressure
  5. additionThe residue was made basic by addition of an aqueous sodium hydroxide solution
  6. extractionthe organic matter was extracted with chloroform
  7. washThe extract was washed with saturated brine and water
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customthe solvent was evaporated under reduced pressure
  10. customThe residue thus obtained
  11. customwas purified by silica gel column chromatography (chloroform:methanol=96:4)