HRID1175054

反应详情

EQUATION

反应方程式

HRID 1175054 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2.45 g of 4-methyl-3-(phenylsulfonyl)-cyclohexan-1-one dissolved in 40 ml of benzene, were added 0.7 ml of 1,2-ethanediol and 0.2 g of paratoluenesulfonic anhydride. The resulting mixture was heated under reflux for 4 hours. After the reaction, a 2M aqueous sodium bicarbonate solution was added and the resulting mixture was extracted with ethyl acetate three times. The combined organic layers were washed with saturated saline, and dried over magnesium sulfate. The solvent was then distilled off under reduced pressure. The residue was recrystallized from ether, whereby 1,1-(ethylenedioxy)-4-methyl-3-(phenylsulfonyl)-cyclohexane was obtained in the form of white crystals (yield: 97%).

WORKUP

后处理

  1. temperatureThe resulting mixture was heated
  2. temperatureunder reflux for 4 hours
  3. customAfter the reaction
  4. extractionthe resulting mixture was extracted with ethyl acetate three times
  5. washThe combined organic layers were washed with saturated saline
  6. dry with materialdried over magnesium sulfate
  7. distillationThe solvent was then distilled off under reduced pressure
  8. customThe residue was recrystallized from ether