HRID1903432

反应详情

EQUATION

反应方程式

HRID 1903432 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. distillationthe solvent is distilled off
  2. dissolutionThe product is dissolved in dichloromethane
  3. filtrationthe insoluble matter is filtered off
  4. distillationthe dichloromethane is distilled off
  5. customto give crude crystals
  6. customRecrystallization from hexane-ether (3:1)