HRID269869

反应详情

EQUATION

反应方程式

HRID 269869 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 1-(4-methoxyphenyl)-4-phenethylpiperazine (165 mg) in 1,2-dichloroethane (1.5 mL), boron tribromide (132 μL) was added under cooling with ice. The temperature was raised to the ambient level, followed by 3 hours' stirring. The reaction mixture was poured in saturated saline solution, rendered weakly alkaline with saturated aqueous sodium hydrogencarbonate solution, and the product was extracted with ethyl acetate. The organic layer was washed with saturated saline solution and dried over anhydrous magnesium sulfate. Distilling the solvent off, the crude product recovered was purified on TLC (developer, chloroform: methanol=15:1) to provide 4-(4-phenethylpiperazin-1-yl)phenol (28 mg).

WORKUP

后处理

  1. temperatureunder cooling with ice
  2. temperatureThe temperature was raised to the ambient level
  3. additionThe reaction mixture was poured in saturated saline solution
  4. extractionthe product was extracted with ethyl acetate
  5. washThe organic layer was washed with saturated saline solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationDistilling the solvent off, the crude product
  8. customrecovered
  9. customwas purified on TLC (developer, chloroform: methanol=15:1)