HRID1756009
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
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
A 70% aqueous ethylamine solution (2.14 g, 33.23 mmol) was added to ethyl 4-(2(4-(2-methylsulfonyloxyethyl)phenyl)ethylamino)-6-ethylpyrimidine-5-carboxylate (0.70 g, 1.66 mmol). The mixture was stirred at 100° C. for 2 hours in a sealed tube and cooled to room temperature. Then water (40 ml) was added to the reaction mixture. The mixture was extracted with methylene chloride and dried over magnesium sulfate. After evaporation of the solvent, the residue was purified by column chromatography on silica gel eluting with ethyl acetate/methanol (=8/2) to give the desired ethyl 4-(2-(4-(2-ethylaminoethyl)phenyl)ethylamino)-6-ethylpyrimidine-5-carboxylate (0.40 g, 65%).
WORKUP
后处理
- temperaturecooled to room temperature
- extractionThe mixture was extracted with methylene chloride
- dry with materialdried over magnesium sulfate
- customAfter evaporation of the solvent
- customthe residue was purified by column chromatography on silica gel eluting with ethyl acetate/methanol (=8/2)