HRID359078

反应详情

EQUATION

反应方程式

HRID 359078 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

p-Chloroaniline (8 g), methanesulfonic acid 2-benzyloxyethyl ester (12.29 g) and sodium hydrogen carbonate (hereinafter, reffered to as sodium bicarbonate) (8.97 g) were dissolved in dioxane (35 ml), suspended and the mixture was heated with stirring for 24 hours. After concentrated under reduced pressure, water and ethyl acetate were added to the mixture and the mixture was separated into layers. The organic layer was washed with water 2 times, and concentrated again under reduced pressure, and the resulting rsidue was subjected to column chromatography on silica gel, and eluted with chloroform/n-hexane [2:1 (v/v)] to give 4-chloro-N-(2-benzyloxyethyl)aniline (4.63 g).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. concentrationAfter concentrated under reduced pressure, water and ethyl acetate
  3. additionwere added to the mixture
  4. customthe mixture was separated into layers
  5. washThe organic layer was washed with water 2 times
  6. concentrationconcentrated again under reduced pressure
  7. washeluted with chloroform/n-hexane [2:1 (v/v)]