HRID1350876

反应详情

EQUATION

反应方程式

HRID 1350876 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a toluene (30 ml) solution of 2-(3-hydroxy-1,1-dimethylpropyl)-5-methoxyphenol (3.0 g, 14.3 mmol) was added catalytic amount of p-toluenesulfonic acid. The stirred mixture was refluxed for 2 hours. The reaction mixture was then quenched with saturated aqueous solution of sodium bicarbonate and then crude products were extracted with ethyl acetate The organic layer was then washed with brine, dried over sodium sulfate. After filtration to separate solvent and sodium sulfate, the solvent was removed under reduced pressure to give a residue, which was applied to a silica gel chromatography column and eluted with ethyl acetate/hexane=1/9 to furnish 2.1 g (75% yield) of the title compound as a colorless oil.

WORKUP

后处理

  1. temperatureThe stirred mixture was refluxed for 2 hours
  2. customThe reaction mixture was then quenched with saturated aqueous solution of sodium bicarbonate
  3. extractioncrude products were extracted with ethyl acetate The organic layer
  4. washwas then washed with brine
  5. dry with materialdried over sodium sulfate
  6. filtrationAfter filtration
  7. customto separate solvent and sodium sulfate
  8. customthe solvent was removed under reduced pressure
  9. customto give a residue, which
  10. washeluted with ethyl acetate/hexane=1/9