HRID261344

反应详情

EQUATION

反应方程式

HRID 261344 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

To a heated (40° C.) solution of 20.1 g (0.97 mole) of n-octadecanethiol in 200 ml of dried 1.2-dimethoxyethane was slowly added under argon 0.07 mole (3.4 g., 50%) of sodium hydride (rinsed with hexane to remove the mineral oil) slurried in 1,2-dimethoxyethane. The reaction mixture was then heated at reflux (85° C.) with stirring for 2 hrs. A solution of 40 g. (0.07 mole) of the nonaethylene glycol monotosylate in 200 ml. 1,2-dimethoxyethane was added dropwise and the reaction mixture allowed to reflux with stirring for 16 hours. The mixture was cooled, insoluble salts were filtered, and the solvent was evaporated to yield a near quantitative yield (0.07 mole) of the thioether.

WORKUP

后处理

  1. washrinsed with hexane
  2. customto remove the mineral oil)
  3. temperatureThe reaction mixture was then heated
  4. temperatureto reflux
  5. stirringwith stirring for 16 hours
  6. temperatureThe mixture was cooled
  7. filtrationinsoluble salts were filtered
  8. customthe solvent was evaporated