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
Methyl bromoacetate (2.1 g) was added to a stirred mixture of N- [2-(4-chlorophenoxy)ethyl]-3-(imidazol-1-yl)propylamine (3.87 g) and anhydrous potassium carbonate (5.73 g) in dry acetone (180 ml). The mixture was stirred and boiled under reflux for 7 hours, then left to stand at ambient temperature for 18 hours then hot filtered. The filtrate was evaporated to dryness and the residue was purified by chromatography on silica using ethyl acetate/triethylamine, 9 to 1 as the mobile phase. The product was obtained as an oil which was dissolved in ether, and extracted into 5M hydrochloric acid. The acid extracts were basified with 5M sodium hydroxide solution and the product extracted into ether to give methyl N-[2-(4-chlorophenoxy)ethyl)-N-[3-(imidazol-1-yl)propyl]glycinate as an oil.
WORKUP
后处理
- temperatureunder reflux for 7 hours
- waitleft
- customThe filtrate was evaporated to dryness
- customthe residue was purified by chromatography on silica
- customThe product was obtained as an oil which
- extractionextracted into 5M hydrochloric acid
- extractionthe product extracted into ether