HRID1903428

反应详情

EQUATION

反应方程式

HRID 1903428 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-(11-hydroxy-1-oxoundecyl)-2,3-dimethoxy-5-methylphenol (14 g) in acetic acid is added 5% palladium-on-carbon (50% hydrate; 3 g) and 70% perchloric acid (0.1 ml), and catalytic reduction is carried out at ambient temperature and atmospheric pressure. After completion of the absorption of hydrogen, the catalyst is filtered off and the filtrate is concentrated under reduced pressure. The residue is extracted with dichloromethane, and the dichloromethane layer is washed with 5% aqueous sodium bicarbonate and dried over anhydrous sodium sulfate. Removal of the solvent by distillation gives a colorless oil of 6-(11-acetoxyundecyl)-2,3-dimethoxy-5-methylphenol (15 g).

WORKUP

后处理

  1. customis carried out at ambient temperature
  2. customAfter completion of the absorption of hydrogen
  3. filtrationthe catalyst is filtered off
  4. concentrationthe filtrate is concentrated under reduced pressure
  5. extractionThe residue is extracted with dichloromethane
  6. washthe dichloromethane layer is washed with 5% aqueous sodium bicarbonate
  7. dry with materialdried over anhydrous sodium sulfate
  8. customRemoval of the solvent
  9. distillationby distillation