HRID1277218
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
In DMF (50 ml) was dissolved N-cyclohexyl-N-methylamine (12.5 g, 0.11 mol), and to the solution were added potassium carbonate (27.6 g, 0.20 mol) and 4-nitrobenzylbromide (21.6 g, 0.10 mol). The mixture was stirred at room temperature for 5 hours. Under reduced pressure, the reaction mixture was concentrated. To the residue was added ethyl acetate, and the mixture was extracted with water. The ethyl acetate layer was washed with saturated sodium chloride solution, dried with MgSO4 and concentrated under reduced pressure. The residue was purified with silica gel column chromatography (ethyl acetate/hexane) to give N-cyclohexyl-N-methyl-N-(4-nitrobenzyl)amine (24.8 g).
WORKUP
后处理
- concentrationUnder reduced pressure, the reaction mixture was concentrated
- additionTo the residue was added ethyl acetate
- extractionthe mixture was extracted with water
- washThe ethyl acetate layer was washed with saturated sodium chloride solution
- dry with materialdried with MgSO4
- concentrationconcentrated under reduced pressure
- customThe residue was purified with silica gel column chromatography (ethyl acetate/hexane)