HRID470328

反应详情

EQUATION

反应方程式

HRID 470328 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 bromoethyl phthalimide 1 (5 mmol) and 2-pyridyl piperazine 2 (5 mmol) in acetonitrile (10 mL) was added potassium carbonate (0.690 g, 5 mmol) and resulting reaction mixture was stirred under reflux. After completion of the reaction, solvent was removed on rotavap and residue was dissolved in chloroform (20 mL). Then washed with water (5 mL) and saturated sodium bicarbonate solution (5 mL), dried over anhydrous sodium sulfate. Filtered and evaporation of solvent gave pyridinylpiperazine ethyl-1H-isoindole-1,3(2H)-dione. Then dissolved in methanol (10 mL), hydrazine hydrate (0.48 mL, 15 mmol) was added and stirred under reflux to give a precipitate. Filtered, washed with methanol (5 mL) and evaporation of solvent gave 2-(4-pyridin-2-ylpiperazin-1-yl)ethanamine 3 which was used as such in the next step.

WORKUP

后处理

  1. customresulting
  2. customreaction mixture
  3. temperatureunder reflux
  4. customAfter completion of the reaction, solvent
  5. customwas removed on rotavap
  6. dissolutionresidue was dissolved in chloroform (20 mL)
  7. washThen washed with water (5 mL) and saturated sodium bicarbonate solution (5 mL)
  8. dry with materialdried over anhydrous sodium sulfate
  9. filtrationFiltered
  10. customevaporation of solvent