HRID1030677

反应详情

EQUATION

反应方程式

HRID 1030677 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In tetrahydrofuran were dissolved and suspended 66.5 g of 2',4',6'-trihydroxyacetophenone and 173.0 g of potassium carbonate, and 56.0 ml of 1-chloro-3-methyl-2-butene was dropped into the solution. The mixture was stirred at room temperature for 2 hours and extracted with dimethyl ether, and the organic layer was washed with a 5% solution of potassium carbonate and then with water. The organic layer was shaken with a saturated solution of sodium chloride, dried with anhydrous sodium sulfate and concentrated under a reduced pressure. Recrystallization from benzene gave 31.8 g (yield=34.0%) of 2',4',6'-trihydroxy-3'-(3-methyl-2-butenyl)acetophenone.

WORKUP

后处理

  1. additionwas dropped into the solution
  2. extractionextracted with dimethyl ether
  3. washthe organic layer was washed with a 5% solution of potassium carbonate
  4. stirringThe organic layer was shaken with a saturated solution of sodium chloride
  5. dry with materialdried with anhydrous sodium sulfate
  6. concentrationconcentrated under a reduced pressure
  7. customRecrystallization from benzene