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
Phytanol (19.5 g) was dissolved in acetic acid (250 ml) and cooled in an ice bath. Chromium trioxide (21.0 g) dissolved in a minimum amount of water was added to the above solution and stirred at room temperature for 18 hours. Ethanol (50 ml) was slowly added to the reaction mixture and stirred for a further 3 hours. Most of solvent was removed and water (250 ml) was added. This solution was extracted with ether (2×200 ml) and the combined ether extract was dried (MgSO4), decolourized with activated charcoal and filtered through a thin flash silica bed. The solvent was removed and the crude product chromatographed on flash silica (1-4% methanol in dichloromethane) to give phytanoic acid as a pale yellow liquid. Yield 7.03 g, 34%.
WORKUP
后处理
- temperaturecooled in an ice bath
- additionwas added to the above solution
- stirringstirred for a further 3 hours
- customMost of solvent was removed
- additionwater (250 ml) was added
- extractionThis solution was extracted with ether (2×200 ml)
- extractionthe combined ether extract
- dry with materialwas dried (MgSO4)
- filtrationfiltered through a thin flash silica bed
- customThe solvent was removed
- customthe crude product chromatographed on flash silica (1-4% methanol in dichloromethane)