HRID1903428
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-(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
- customis carried out at ambient temperature
- customAfter completion of the absorption of hydrogen
- filtrationthe catalyst is filtered off
- concentrationthe filtrate is concentrated under reduced pressure
- extractionThe residue is extracted with dichloromethane
- washthe dichloromethane layer is washed with 5% aqueous sodium bicarbonate
- dry with materialdried over anhydrous sodium sulfate
- customRemoval of the solvent
- distillationby distillation