HRID974994

反应详情

EQUATION

反应方程式

HRID 974994 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

32.27 g of homopiperazine, 13.2 g of 2-(3,4-dimethoxyphenyl)ethyl chloride and 71.3 g of potassium carbonate were added to 500 ml of acetonitrile. The obtained mixture was heated under reflux for 20 hours, cooled and filtered. The filtrate was concentrated under a reduced pressure to obtain a residue. This residue was extracted with ether thrice. The extracts were combined, dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated under a reduced pressure. The obtained residue was purified by silica gel column chromatography (solvent: chloroform/methanol/isopropylamine (100:10:1)) to obtain 13.40 g of the title compound as a yellow oil (yield: 77%).

WORKUP

后处理

  1. temperatureThe obtained mixture was heated
  2. temperatureunder reflux for 20 hours
  3. temperaturecooled
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated under a reduced pressure
  6. customto obtain a residue
  7. extractionThis residue was extracted with ether thrice
  8. dry with materialdried over anhydrous sodium sulfate
  9. filtrationfiltered
  10. concentrationThe filtrate was concentrated under a reduced pressure
  11. customThe obtained residue was purified by silica gel column chromatography (solvent: chloroform/methanol/isopropylamine (100:10:1))