HRID441057

反应详情

EQUATION

反应方程式

HRID 441057 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6.88 g of 5,7-dihydroxy-2-methylthiochromone (30.35 mmol), 12.56 g of potassium carbonate (91.05 mmol), 6.07 ml of isopropyl iodide (60.70 mmol) and 150 ml DMF were stirred at 60° C. for 30 minutes. After addition of water, the reaction solution was extracted twice with ethyl acetate, and the organic layer was washed with saturated NaCl water and was then dried over sodium sulfate anhydride. The solvent was distilled off under reduced pressure, and the crude product was purified by flash column chromatography (hexane : ethyl acetate=4 : 1), to give 6.71 g of 5-hydroxy-7-isopropoxy-2-methylthiochromone (83% yield).

WORKUP

后处理

  1. extractionthe reaction solution was extracted twice with ethyl acetate
  2. washthe organic layer was washed with saturated NaCl water
  3. dry with materialwas then dried over sodium sulfate anhydride
  4. distillationThe solvent was distilled off under reduced pressure
  5. customthe crude product was purified by flash column chromatography (hexane : ethyl acetate=4 : 1)