HRID390005

反应详情

EQUATION

反应方程式

HRID 390005 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-(4-Methoxyphenyl)piperazine dihydrochloride (1.85 g, 6.976 mmol) was dissolved in methylene chloride. After adding triethylamine (1.9 mL, 13.952 mmol) dropwise at 0° C. and then dissolving, the mixture was stirred for 30 minutes. After adding 3-chloropropionyl chloride (0.67 mL, 6.976 mmol), the reaction solution was stirred at room temperature for 1 hour. After adding methanol, the reaction solution was extracted with methylene chloride. The organic layer was dried with desiccant and then filtered. The filtrate was concentrated and purified by column chromatography (EtOAc/hexane, 4:1). A target compound (1.76 g, 6.224 mmol, 89.3%) was yielded as white solid.

WORKUP

后处理

  1. dissolutiondissolving
  2. stirringthe reaction solution was stirred at room temperature for 1 hour
  3. extractionthe reaction solution was extracted with methylene chloride
  4. customThe organic layer was dried with desiccant and
  5. filtrationthen filtered
  6. concentrationThe filtrate was concentrated
  7. custompurified by column chromatography (EtOAc/hexane, 4:1)