HRID2228415

反应详情

EQUATION

反应方程式

HRID 2228415 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. temperaturecooled in an ice bath
  2. additionwas added to the above solution
  3. stirringstirred for a further 3 hours
  4. customMost of solvent was removed
  5. additionwater (250 ml) was added
  6. extractionThis solution was extracted with ether (2×200 ml)
  7. extractionthe combined ether extract
  8. dry with materialwas dried (MgSO4)
  9. filtrationfiltered through a thin flash silica bed
  10. customThe solvent was removed
  11. customthe crude product chromatographed on flash silica (1-4% methanol in dichloromethane)