HRID358904

反应详情

EQUATION

反应方程式

HRID 358904 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

350 ml (2.8 moles) of ethyl methacrylate were added to a solution of 150 g (1.4 moles) of benzylamine dissolved in 400 ml of ethanol. The mixture was heated under reflux for 4 hours, and then 175 ml (1.4 mole) of ethyl methacrylate were added to it, after which it was heated under reflux for 24 hours. The solvent and the unreacted materials were then removed from the mixture by evaporation under reduced pressure. The residue was purified by column chromatography through silica gel eluted with a 1:1 by volume mixture of ethyl acetate and toluene, to afford 98.0 g of N-(2-ethoxycarbonylpropyl)benzylamine as a red oil.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 4 hours
  3. temperatureafter which it was heated
  4. temperatureunder reflux for 24 hours
  5. customThe solvent and the unreacted materials were then removed from the mixture by evaporation under reduced pressure
  6. customThe residue was purified by column chromatography through silica gel
  7. washeluted with a 1:1 by volume mixture of ethyl acetate and toluene