HRID1903432
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 (200 ml) of 6-(12-acetoxydodecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone (4.4 g) in methanol is added concentrated hydrochloric acid (0.1 ml) and the mixture is allowed to stand at room temperature for 12 hours. To this reaction mixture is added sodium bicarbonate (0.2 g), and the solvent is distilled off. The product is dissolved in dichloromethane, the insoluble matter is filtered off and the dichloromethane is distilled off to give crude crystals. Recrystallization from hexane-ether (3:1) gives orange-yellow needles of 6-(12-hydroxydodecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone (3.8 g). m.p. 63° C.
WORKUP
后处理
- distillationthe solvent is distilled off
- dissolutionThe product is dissolved in dichloromethane
- filtrationthe insoluble matter is filtered off
- distillationthe dichloromethane is distilled off
- customto give crude crystals
- customRecrystallization from hexane-ether (3:1)