HRID974994
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe obtained mixture was heated
- temperatureunder reflux for 20 hours
- temperaturecooled
- filtrationfiltered
- concentrationThe filtrate was concentrated under a reduced pressure
- customto obtain a residue
- extractionThis residue was extracted with ether thrice
- dry with materialdried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationThe filtrate was concentrated under a reduced pressure
- customThe obtained residue was purified by silica gel column chromatography (solvent: chloroform/methanol/isopropylamine (100:10:1))