反应详情

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

1. extractionThe reaction mixture is subjected to extraction with dichloromethane
2. washthe organic layer is washed with water
3. dry with materialdried over magnesium sulfate
4. distillationThe solvent is distilled off
5. customto thereby leave crude crystals
6. customThe product is recrystallized from hexane