HRID1788673

反应详情

EQUATION

反应方程式

HRID 1788673 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To N-(3-chloropropionyl)-3,4-methylenedioxyaniline (2.0 g) dissolved in N,N-dimethylformamide (20 ml) were added N-phenylpiperazine (1.6 g) and triethylamine (3 ml) and the mixture was stirred at 80° C. for 20 hours in a nitrogen atmosphere. The reaction mixture was evaporated in vacuo and to the residue were added ethyl acetate and 2N sodium hydroxide solution. After the aqueous layer was removed, the ethyl acetate layer was washed twice with water and dried over anhydrous sodium sulfate. The ethyl acetate was then distilled off and the residual solid was recrystallized from ethanol to give N-[3-(4-phenyl-1-piperazinyl)propionyl]-3,4-methylenedioxyaniline (3.4 g, 90% yield).

WORKUP

后处理

  1. customThe reaction mixture was evaporated in vacuo and to the residue
  2. additionwere added ethyl acetate and 2N sodium hydroxide solution
  3. customAfter the aqueous layer was removed
  4. washthe ethyl acetate layer was washed twice with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationThe ethyl acetate was then distilled off
  7. customthe residual solid was recrystallized from ethanol