HRID356227

反应详情

EQUATION

反应方程式

HRID 356227 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

55.7 g (0.34 mol) of N-ethyl-N-(2-hydroxylethyl)aniline was dissolved in 250 ml of anhydrous tetrahydrofuran, and 162 ml (1.2-fold equivalent weight) of a 2.5M hexane solution n-butyllithium was dropwise added thereto over a period of 30 minutes at 0° C. in an atmosphere of argon, followed by stirring at 0° C. for 30 minutes. Next, to the reaction solution obtained, 30.0 g (1.09-fold equivalent weight) of methoxymethyl chloride was dropwise added, and the solution was heated and refluxed for 12 hours, followed by cooling. The precipitate formed was removed by filtration, and thereafter the filtrate obtained was concentrated under reduced pressure. The oily residue thus obtained was distilled under reduced pressure to obtain 63 g of N-ethyl-N-[2-(methoxymethyl)oxyethyl]aniline (yield: 89%).

WORKUP

后处理

  1. customNext, to the reaction solution obtained
  2. temperaturethe solution was heated
  3. temperaturerefluxed for 12 hours
  4. temperatureby cooling
  5. customThe precipitate formed
  6. customwas removed by filtration
  7. customthe filtrate obtained
  8. concentrationwas concentrated under reduced pressure
  9. customThe oily residue thus obtained
  10. distillationwas distilled under reduced pressure