HRID1030680

反应详情

EQUATION

反应方程式

HRID 1030680 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 250 ml of anhydrous tetrahydrofuran was dissolved 50.0 g of 2',4',6'-trihydroxyacetophenone, and 123.1 g of anhydrous potassium carbonate was added to the solution and the mixture was stirred at room temperature for 30 minutes. Then, 37.2 g of 1-chloro3-methyl-2-butene was added dropwise to the mixture over a period of 20 minutes and reaction was carried out at room temperature for 24 hours. After the reaction, the reaction mixture was extracted with 2 l of ethyl acetate and the solvent was removed from the ethyl acetate layer by distillation, and the residue was recrystallized from a benzene/petroleum ether mixed solvent to obtain 38.6 g (yield=55.0%) of 2',4',6'-trihydroxy-3'-(3-methyl-2-butenyl)acetophenone in the form of a yellow prism.

WORKUP

后处理

  1. additionwas added to the solution
  2. customreaction
  3. waitwas carried out at room temperature for 24 hours
  4. customAfter the reaction
  5. extractionthe reaction mixture was extracted with 2 l of ethyl acetate
  6. customthe solvent was removed from the ethyl acetate layer by distillation
  7. customthe residue was recrystallized from a benzene/petroleum ether mixed solvent