HRID1029617

反应详情

EQUATION

反应方程式

HRID 1029617 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Acetylpyridine (10 g), ethylene glycol (50 ml) and p-toluenesulfonic acid (0.5 g) were dissolved in toluene and the solution was refluxed at 150° C. for 1 day with the by-product water being constantly removed. After cooling, saturated aqueous sodium hydrogen carbonate and toluene were added and the mixture was stirred and allowed to stand. The aqueous layer was separated and extracted with 2 portions of toluene. The toluene layers were combined, washed sequentially with saturated aqueous sodium hydrogen carbonate, water and aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate. Finally the solvent was distilled off under reduced pressure to give 2-methyl-2-(pyridin-3-yl)-1,3-dioxolane (13.6 g).

WORKUP

后处理

  1. customconstantly removed
  2. temperatureAfter cooling
  3. additionsaturated aqueous sodium hydrogen carbonate and toluene were added
  4. customThe aqueous layer was separated
  5. extractionextracted with 2 portions of toluene
  6. washwashed sequentially with saturated aqueous sodium hydrogen carbonate, water and aqueous sodium chloride solution
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationFinally the solvent was distilled off under reduced pressure