HRID1277218

反应详情

EQUATION

反应方程式

HRID 1277218 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationUnder reduced pressure, the reaction mixture was concentrated
  2. additionTo the residue was added ethyl acetate
  3. extractionthe mixture was extracted with water
  4. washThe ethyl acetate layer was washed with saturated sodium chloride solution
  5. dry with materialdried with MgSO4
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified with silica gel column chromatography (ethyl acetate/hexane)