HRID269880

反应详情

EQUATION

反应方程式

HRID 269880 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 1-(3-chloro-4-methoxymethoxyphenyl)-4-phenethyl-piperazine (214 mg), 2-propanol (1 mL) and tetrahydrofuran (1 mL) were added, followed by cooling with ice and addition of conc. hydrochloric acid (0.5 mL). Raising the temperature back to the ambient level, the mixture was stirred for 4.5 hours. 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. The solvent was distilled off and the resulting crude product was purified on TLC (developer, chloroform: acetone=5:1) to provide 2-chloro-4-(4-phenethylpiperazin-1-yl)phenol (93 mg).

WORKUP

后处理

  1. temperatureRaising the temperature back to the ambient level
  2. additionThe reaction mixture was poured in saturated saline solution
  3. extractionthe product was extracted with ethyl acetate
  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 resulting crude product was purified on TLC (developer, chloroform: acetone=5:1)