反应详情

To a solution of 6-(11-acetoxyundecyl)-2,3-dimethoxy-5-methylphenol (8 g) in N,N-dimethylformamide (400 ml) are added potassium nitrosodisulfonate (24 g), water (400 ml), methanol (30 ml) and monopotassium phosphate (1.0 g). The mixture is stirred at room temperature for 28 days. The product is extracted with dichloromethane and the dichloromethane layer is washed with water and dried over anhydrous magnesium sulfate. The solvent is then distilled off and the resultant crude crystals are recrystallized from hexane. The above procedure yields 6-(11-acetoxyundecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone (6.4 g) as orange-yellow needles, m.p. 41° C.

1. extractionThe product is extracted with dichloromethane
2. washthe dichloromethane layer is washed with water
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationThe solvent is then distilled off
5. customthe resultant crude crystals are recrystallized from hexane