HRID1418255

反应详情

EQUATION

反应方程式

HRID 1418255 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Triiodomesitylene (19.5 g, 39 mmol) was added to glacial acetic acid (200 ml) containing acetic anhydride (400 ml) and concentrated sulfuric acid (40 ml). Solid potassium permanganate (24.6 g, 156 mmol) was then added in small portions over a period of 3 h. After stirring for 16 h, the solvent was evaporated and water (200 ml) was added. The aqueous suspension was extracted with dichloromethane (250 ml) and the organic phase was washed with water (3×50 ml), dried (MgSO4) and evaporated. The solid residue was suspended in acetone and the white crystalline product was collected by filtration. Yield: 9.3 g (35%).

WORKUP

后处理

  1. customthe solvent was evaporated
  2. additionwater (200 ml) was added
  3. extractionThe aqueous suspension was extracted with dichloromethane (250 ml)
  4. washthe organic phase was washed with water (3×50 ml)
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. filtrationthe white crystalline product was collected by filtration