HRID637892
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 6-(11-acetoxyundecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone (4.2 g) in methanol (200 ml) is added concentrated sulfuric acid (0.1 ml) and the mixture is kept standing at room temperature for 12 hours. To a reaction mixture is added potassium hydrogencarbonate (0.2 g) and the solvent is distilled off. The resultant is dissolved in dichloromethane and insolubles are filtered off. Dichloromethane is distilled off to leave crude crystals. Recrystallization from hexane-ether (3:1) gives 6-(11-hydroxyundecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone (3.6 g) as orange-yellow needles. m.p.: 57° C.
WORKUP
后处理
- distillationthe solvent is distilled off
- dissolutionThe resultant is dissolved in dichloromethane
- filtrationinsolubles are filtered off
- distillationDichloromethane is distilled off
- customto leave crude crystals
- customRecrystallization from hexane-ether (3:1)