HRID35276

反应详情

EQUATION

反应方程式

HRID 35276 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

150 g of potassium carbonate and 4 g of finely powdered potassium iodide are added to a solution of 112 g (0.6 mole) of 4-phenoxyphenol and 157.6 g (0.8 mole) of bromoacetaldehyde diethyl acetal in 480 ml of dimethylformamide, and the batch is heated, under nitrogen, for 14 hours at 150° C. The salts are then removed by filtration from the reaction solution, and most of the dimethylformamide is distilled off in a water jet vacuum. The residue is dissolved in ether and the resultant solution is washed twice with water, three times with 20% potassium hydroxide solution and again with water. The ethereal solution is then dried over sodium sulfate and the ether is distilled off entirely. The resultant 4-phenoxyphenoxyacetaldehyde diethyl acetal is used without further purification for the preparation of the free aldehyde.

WORKUP

后处理

  1. customThe salts are then removed by filtration from the reaction solution
  2. distillationmost of the dimethylformamide is distilled off in a water jet vacuum
  3. dissolutionThe residue is dissolved in ether
  4. washthe resultant solution is washed twice with water, three times with 20% potassium hydroxide solution and again with water
  5. dry with materialThe ethereal solution is then dried over sodium sulfate
  6. distillationthe ether is distilled off entirely
  7. customThe resultant 4-phenoxyphenoxyacetaldehyde diethyl acetal is used without further purification for the preparation of the free aldehyde