HRID269871

反应详情

EQUATION

反应方程式

HRID 269871 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
210 °C

PROCEDURE

实验过程

A mixture of 1-(4-methoxy-3-methylphenyl)-4-phenethyl-piperazine (327 mg) and pyridinium chloride (731 mg) was heated to 210° C. and stirred for an hour. The reaction liquid was diluted with 1 mL of toluene, and to which saturated saline solution was added. Further adding saturated aqueous sodium hydrogencarbonate solution to render the system weakly alkaline, the product was extracted with ethyl acetate-tetrahydrofuran (1:1). The organic layer was washed with saturated saline solution and dried over anhydrous magnesium sulfate. The solvent was distilled off and the remaining crude product was purified on TLC (developer, chloroform: methanol=15:1) to provide 2-methyl-4-(4-phenethylpiperazin-1-yl)phenol (141 mg).

WORKUP

后处理

  1. customThe reaction liquid
  2. additionto which saturated saline solution was added
  3. extractionthe product was extracted with ethyl acetate-tetrahydrofuran (1:1)
  4. washThe organic layer was washed with saturated saline solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled off
  7. customthe remaining crude product was purified on TLC (developer, chloroform: methanol=15:1)