HRID2052806

反应详情

EQUATION

反应方程式

HRID 2052806 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of piperazine (350 mmol), KOH (100 mmol) and hexadecyl-trimethyl ammonium bromide (CTAB, 1 mmol) in water (18 ml) was heated to get a solution. Thereafter, benzyl chloride (100 mmol) in 140 ml of benzene was added to the solution dropwise at 70° C., and refluxed for 1 h. The organic layer was washed with water and saline, dried (MgSO4), filtered and evaporated, the residue was dissolved by 50 ml of ethanol and adjusted to a PH of 2 by HCl/C2H5OH (5N), the resulting precipitate was recrystallized from ethanol to obtain N-benzyl piperazine dihydrochloride (55-86%).

WORKUP

后处理

  1. temperaturewas heated
  2. customto get a solution
  3. temperaturerefluxed for 1 h
  4. washThe organic layer was washed with water and saline
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customevaporated
  8. dissolutionthe residue was dissolved by 50 ml of ethanol
  9. customthe resulting precipitate was recrystallized from ethanol