HRID1744499

反应详情

EQUATION

反应方程式

HRID 1744499 的结构方程式

PROCEDURE

实验过程

2-Chloro-5-nitrobenzonitrile (15 g) and piperazinoethanol (16 g) were added to ethanol (100 ml) and the mixture was stirred at a refluxing temperature for 1 h. The solvent was evaporated under reduced pressure. To the residue was added aqueous sodium hydroxide solution and the mixture was extracted with chloroform. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate, after which the solvent was evaporated under reduced pressure. To the residue diisopropyl ether was added to allow crystallization. The crystals were recrystallized from hydrous ethanol to give 5-nitro-2-(2-hydroxyethylpiperazin-1-yl)benzonitrile (18.7 g), melting point 100–102° C.

WORKUP

后处理

  1. customThe solvent was evaporated under reduced pressure
  2. additionTo the residue was added aqueous sodium hydroxide solution
  3. extractionthe mixture was extracted with chloroform
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customafter which the solvent was evaporated under reduced pressure
  7. additionTo the residue diisopropyl ether was added
  8. customcrystallization
  9. customThe crystals were recrystallized from hydrous ethanol