HRID1291688

反应详情

EQUATION

反应方程式

HRID 1291688 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a 2-l flask equipped with a stirrer, a dropping funnel, a nitrogen gas inlet tube and a distillation apparatus, 743.2 g (8.34 mol) of 3-methoxypropylamine (5-a) and 150 ml of ethanol were charged, followed by the dropwise addition of 165.9 g (0.56 mol) of hexadecyl glycidyl ether (4-a) over 3 hours while stirring under heating to 80° C. in a nitrogen atmosphere. After the completion of the dropwise addition, stirring was conducted for further 2 hours at 80° C. From the reaction mixture, ethanol and excessive 3-methoxypropylamine were distilled off by heating under reduced pressure. The residue was purified by chromatography on a silica gel column, whereby 196.5 g of the title compound (6-a) were obtained in the form of a white solid (yield: 91% relative to hexadecyl glycidyl ether).

WORKUP

后处理

  1. customTo a 2-l flask equipped with a stirrer, a dropping funnel, a nitrogen gas inlet tube
  2. additionAfter the completion of the dropwise addition
  3. stirringstirring
  4. distillationFrom the reaction mixture, ethanol and excessive 3-methoxypropylamine were distilled off
  5. temperatureby heating under reduced pressure
  6. customThe residue was purified by chromatography on a silica gel column