HRID1122

反应详情

EQUATION

反应方程式

HRID 1122 的结构方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A 500-ml flask equipped with a stirrer was charged with 160 g (1.5 mol) of benzylamine, to which 29 g (0.11 mol) of 1,2-epoxyoctadecane were added dropwise over 3 hours while stirring at 100° C. Stirring was conducted further for 12 hours at 100° C. Benzyl alcohol was distilled off under reduced pressure, and the residue was charged into a 500-ml autoclave, to which 300 ml of ethanol and 10 g of 5% Pd/C were added to conduct hydrogenolysis for 48 hours at room temperature under a hydrogen pressure of 5 atm. After the catalyst was separated by filtration, the filtrate was concentrated under reduced pressure, and the residue was recrystallized from hexane, thereby obtaining 26.1 g (yield: 83%) of the title compound (IIh-7).

WORKUP

后处理

  1. customA 500-ml flask equipped with a stirrer
  2. additionwere added dropwise over 3 hours
  3. stirringStirring
  4. distillationBenzyl alcohol was distilled off under reduced pressure
  5. additionthe residue was charged into a 500-ml autoclave, to which 300 ml of ethanol and 10 g of 5% Pd/C
  6. additionwere added
  7. customfor 48 hours
  8. customat room temperature
  9. customAfter the catalyst was separated by filtration
  10. concentrationthe filtrate was concentrated under reduced pressure
  11. customthe residue was recrystallized from hexane