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
0.90 g of 1-methyl-7-nitro-1,2,3,4-tetrahydroisoquinoline was dissolved in 20 ml of ethanol, and 1.97 g of sodium bicarbonate, 2.55 g of ethyl bromopropionate, and a catalytic amount of potassium iodide were added to the solution. The solution was heated overnight under ref lux with stirring, and extracted with ethyl acetate. After washing with water and saturated aqueous solution of sodium chloride, the solution was dried with anhydrous sodium sulfate. The desiccant was separated by filtration, and the filtrate was purified by silica gel column chromatography to obtain 0.90 g of 2-[2-(ethoxycarbonyl)ethyl]-1-methyl-7-nitro-1,2,3,4-tetrahydroisoquinoline, which was an oily product (yield: 65%).
WORKUP
后处理
- temperatureThe solution was heated overnight under ref lux
- extractionextracted with ethyl acetate
- washAfter washing with water and saturated aqueous solution of sodium chloride
- dry with materialthe solution was dried with anhydrous sodium sulfate
- customThe desiccant was separated by filtration
- customthe filtrate was purified by silica gel column chromatography