反応 #63554

反応方程式

potassium carbonate

potassium iodide

4-phenoxyphenol

bromoacetaldehyde diethyl acetal

→

4-phenoxyphenoxyacetaldehyde diethyl acetal

溶媒

dimethylformamide

反応条件

後処理

1. 1
   その他The salts are then removed by filtration from the reaction solution
2. 2
   workup.DISTILLATIONmost of the dimethylformamide is distilled off in a water jet vacuum
3. 3
   workup.DISSOLUTIONThe residue is dissolved in ether
4. 4
   洗浄the resultant solution is washed twice with water, three times with 20% potassium hydroxide solution and again with water
5. 5
   乾燥The ethereal solution is then dried over sodium sulfate
6. 6
   workup.DISTILLATIONthe ether is distilled off entirely
7. 7
   その他The resultant 4-phenoxyphenoxyacetaldehyde diethyl acetal is used without further purification for the preparation of the free aldehyde

実験手順

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.

出典