HRID1079392

反应详情

EQUATION

反应方程式

HRID 1079392 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of p-fluoronitrobenzene (31.8 ml) in dimethylformamide (200 ml) was ice-cooled and to this was added piperidine (60 ml) dropwise, followed by stirring with ice cooling for 2 hours. After the solvent was distilled off, the residual oily product was dissolved in ethyl acetate ester (200 ml), followed by washing in turn with aqueous saturated solution of sodium bicarbonate and water. Then, the solution was dried over anhydrous magnesium sulfate. After the solvent was distilled off, the residue was recrystallized from n-hexane to obtain N-(4-nitrophenyl)piperidine as yellow crystals (52.8 g).

WORKUP

后处理

  1. temperaturecooled
  2. distillationAfter the solvent was distilled off
  3. dissolutionthe residual oily product was dissolved in ethyl acetate ester (200 ml)
  4. washby washing in turn with aqueous saturated solution of sodium bicarbonate and water
  5. dry with materialThen, the solution was dried over anhydrous magnesium sulfate
  6. distillationAfter the solvent was distilled off
  7. customthe residue was recrystallized from n-hexane