HRID1903431

反应详情

EQUATION

反应方程式

HRID 1903431 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution (300 ml) of 6-(12-acetoxydodecyl)-2,3-dimethoxy-5-methylphenol (6.1 g) in dimethylformamide are added potassium nitrosodisulfonate (18 g), water (300 ml), methanol (50 ml) and potassium dihydrogen phosphate (0.5 g), and the mixture is stirred at room temperature for 30 days. The product is extracted with dichloromethane, and the organic layer is washed with water and dried over anhydrous magnesium sulfate. The solvent is distilled off to give crude crystals. This product is recrystallized from hexane to give orange-yellow needles of 6-(12-acetoxydodecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone (4.8 g). m.p. 47° C.

WORKUP

后处理

  1. extractionThe product is extracted with dichloromethane
  2. washthe organic layer is washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationThe solvent is distilled off
  5. customto give crude crystals
  6. customThis product is recrystallized from hexane