HRID1257943

反应详情

EQUATION

反应方程式

HRID 1257943 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Toluene (200 ml) and pyrrolidine (90 ml) were added to 4-(1,4-dioxaspiro[4.5]decan-8-yl)cyclohexanone (100 g) in a reaction vessel equipped with a Dean-Stark apparatus under an atmosphere of nitrogen. The mixture was refluxed for 3 hours while the water formed was removed by a Dean-Stark apparatus. After the reaction mixture had been cooled to a room temperature, it was washed with brine, and dried over anhydrous magnesium sulfate. The toluene was distilled off to give 1-(4-(1,4-dioxaspiro[4.5]decan-8-yl)cyclohex-1-enyl)pyrrolidine (105.8 g).

WORKUP

后处理

  1. customequipped with a Dean-Stark apparatus under an atmosphere of nitrogen
  2. customformed
  3. customwas removed by a Dean-Stark apparatus
  4. washit was washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationThe toluene was distilled off