HRID637889

反应详情

EQUATION

反应方程式

HRID 637889 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 6-(12-acetoxydodecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone (4.4 g) in methanol (200 ml) is added concentrated hydrochloric acid (0.1 ml) and the mixture is kept standing at room temperature for 12 hours. To the reaction mixture is added sodium hydrogen carbonate (0.2 g), and the solvent is distilled off. The residue is dissolved in dichloromethane and the insoluble materials are filtered off. Dichloromethane is distilled off to thereby leave crude crystals. Recrystallization from hexane-ether (3:1) gives 6-(12-hydroxydodecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone (3.8 g) as orange-yellow needles. Melting point: 63° C.

WORKUP

后处理

  1. distillationthe solvent is distilled off
  2. dissolutionThe residue is dissolved in dichloromethane
  3. filtrationthe insoluble materials are filtered off
  4. distillationDichloromethane is distilled off
  5. customto thereby leave crude crystals
  6. customRecrystallization from hexane-ether (3:1)