HRID646195

反应详情

EQUATION

反应方程式

HRID 646195 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

21.56 g of 4-(2,4-dichlorophenoxy)-3-hydroxybenzonitrile, 14.2 g of chloroacetone, 12.8 g of potassium carbonate and 170 mg of potassium iodide are dissolved in 300 ml of acetone and boiled under reflux for 5 h. After cooling, the precipitate is filtered, concentrated by evaporation, redissolved in ethylacetate and washed with a 1N aqueous solution of sodium hydroxide, water, a 1N aqueous solution of hydrogen chloride and finally with brine. The organic phase is dried over magnesium sulfate and evaporated. The residue is recrystallized from ethylacetate/hexane to yield 4-(2,4-dichlorophenoxy)-3-(2-oxopropoxy)-benzonitrile.

WORKUP

后处理

  1. temperatureunder reflux for 5 h
  2. temperatureAfter cooling
  3. filtrationthe precipitate is filtered
  4. concentrationconcentrated by evaporation
  5. dissolutionredissolved in ethylacetate
  6. washwashed with a 1N aqueous solution of sodium hydroxide, water
  7. dry with materialThe organic phase is dried over magnesium sulfate
  8. customevaporated
  9. customThe residue is recrystallized from ethylacetate/hexane