反应 #1681097

反应方程式

water

3-[(6-bromohexyloxy)methyl]-3-ethyloxetane

4-hydoxybenzoic acid

potassium carbonate

→

4-[6-(3-ethyloxetane-3-ylmethoxy) hexyloxy]benzoic acid

收率 66.4%

溶剂

dimethylforamide

反应条件

后处理

1. 1
   其他First stage: A solution prepared
2. 2
   萃取was extracted with 4 L of toluene
3. 3
   洗涤The organic layer was washed with water
4. 4
   workup.DISTILLATIONthe solvent was distilled off
5. 5
   workup.ADDITIONAdded to the resulting residue
6. 6
   温度the mixture was refluxed for 4 hours
7. 7
   workup.DISTILLATIONEthanol 1 L was distilled off at an atmospheric pressure
8. 8
   其他to obtain a slurry
9. 9
   过滤The slurry was filtered
10. 10
    其他dried

实验过程

First stage: A solution prepared by dissolving 500 g of 3-[(6-bromohexyloxy)methyl]-3-ethyloxetane, 297 g of 4-hydoxybenzoic acid and 490 g of potassium carbonate in 3 L of dimethylforamide was stirred at 90° C. for 8 hours. After adding 4 L of water to the reaction mixture, it was extracted with 4 L of toluene. The organic layer was washed with water, and then the solvent was distilled off. Added to the resulting residue were 200 g of sodium hydroxide, 1 L of water and 2.5 L of ethanol, and the mixture was refluxed for 4 hours. Ethanol 1 L was distilled off at an atmospheric pressure, and then the solution was acidified by hydrochloric acid to obtain a slurry. The slurry was filtered and dried to thereby obtain 400 g of 4-[6-(3-ethyloxetane-3-ylmethoxy) hexyloxy]benzoic acid (melting point: 58.5° C.).

来源