HRID427449

反应详情

EQUATION

反应方程式

HRID 427449 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of N-(4-pyridyl)piperazine (815 mg), 4-fluorobenzophenone (1.2 g) and powdered potassium carbonate (912 mg) was stirred at 95° C. in DMSO (10 ml) overnight. The solution was poured into water (150 ml) and extracted with dichloromethane (3×50 ml). The dichloromethane extracts were combined, washed with water, dried (Na2SO4) and evaporated. The residue was purified by chromatography on alumina (ICN Alumina N 32-63) using 1% methanol in dichloromethane as eluant to give a solid. The solid was recrystallised from a mixture of ethyl acetate/isohexane to give 1-(4-benzoylphenyl)-4-(4-pyridyl)piperazine (450 mg) as a solid. m.p.136-137° C.

WORKUP

后处理

  1. extractionextracted with dichloromethane (3×50 ml)
  2. washwashed with water
  3. dry with materialdried (Na2SO4)
  4. customevaporated
  5. customThe residue was purified by chromatography on alumina (ICN Alumina N 32-63)
  6. customto give a solid
  7. customThe solid was recrystallised from a mixture of ethyl acetate/isohexane