HRID2399770

反应详情

EQUATION

反应方程式

HRID 2399770 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 0.135 g (0.218 mmol) of 80% magnesium monoperoxyphthalate acid (MMPP) and 2 ml iso-propyl alcohol was added enough water (0.20 ml) to just dissolve the solid. This solution was added to a solution of 0.058 g (0.182 mmol) of 6-[2-(2,6,6-trimethylcyclohex-1-enyl)ethynyl]-2-naphthoic acid (Compound 4) in 1 ml iso-propyl alcohol and stirred at ambient temperature for 3 days. The solution was treated with 2 ml of brine and extracted with 3×10 ml ethyl acetate. The organic extracts were combined and washed with 5 ml saturated aqueous NaCl and dried (MgSO4). The solvent was removed in-vacuo and the residue purified by flash chromatography (SiO2, 75:25 ethyl acetate in hexanes) to give the title compound as a white solid

WORKUP

后处理

  1. dissolutionto just dissolve the solid
  2. extractionextracted with 3×10 ml ethyl acetate
  3. washwashed with 5 ml saturated aqueous NaCl
  4. dry with materialdried (MgSO4)
  5. customThe solvent was removed in-vacuo
  6. customthe residue purified by flash chromatography (SiO2, 75:25 ethyl acetate in hexanes)