HRID266060

反应详情

EQUATION

反应方程式

HRID 266060 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 1-(4-methoxyphenyl)piperazine dihyclrochloride (0.050 mol), 1-chloro-4-nitrobenzene (0.050 mol) and potassium carbonate (10.0 g) in N,N-dimethylform-amide (100 ml) was stirred and refluxed overnight. The reaction mixture was diluted with water and extracted twice with trichloromethane. The organic layers were combined, dried (MgSO4), filtered and evaporated in vacuum. The residue was successively triturated in 4-methyl-2-pentanone and recrystallized from 1,4-dioxane. The product was filtered off and dried, yielding 10.5 g (67%) of 1-(4-methoxyphenyl)-4-(4-nitrophenyl)-piperazine; mp. 195.1° C. (interm. 1).

WORKUP

后处理

  1. temperaturerefluxed overnight
  2. extractionextracted twice with trichloromethane
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customevaporated in vacuum
  6. customThe residue was successively triturated in 4-methyl-2-pentanone
  7. customrecrystallized from 1,4-dioxane
  8. filtrationThe product was filtered off
  9. customdried