HRID1030684

反应详情

EQUATION

反应方程式

HRID 1030684 的结构方程式

PROCEDURE

实验过程

In 160 ml of anhydrous tetrahydrofuran were dissolved 18.4 g of the so-obtained 2',4',6'-trihydroxy3'-(2-propenyl)acetophenone and 57.1 g of N,N-diisopropylethylamine, and 28.4 g of chrolomethyl methyl ether was added to the solution under ice cooling and the reaction mixture was stirred under ice cooling for 1 hour, and further, stirred at room temperature for 4 hours to effect a reaction. The reaction mixture was extracted with diethyl ether and filtered, and the solvent was removed from the filtrate by distillation. The obtained residue was subjected to the silica gel column chromatography [eluting solvent=n-hexane/ethyl acetate (7/1)] to obtain 24.8 g (yield=94.7%) of 2'-hydroxy-4',6'-bismethoxymethoxy-3'-(2-propenyl)acetophenone in the form of a colorless oil.

WORKUP

后处理

  1. additionwas added to the solution under ice cooling
  2. stirringfurther, stirred at room temperature for 4 hours
  3. customa reaction
  4. extractionThe reaction mixture was extracted with diethyl ether
  5. filtrationfiltered
  6. customthe solvent was removed from the filtrate by distillation
  7. washThe obtained residue was subjected to the silica gel column chromatography [eluting solvent=n-hexane/ethyl acetate (7/1)]