反应详情

温度

90 °C

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.).

1. customFirst stage: A solution prepared
2. extractionwas extracted with 4 L of toluene
3. washThe organic layer was washed with water
4. distillationthe solvent was distilled off
5. additionAdded to the resulting residue
6. temperaturethe mixture was refluxed for 4 hours
7. distillationEthanol 1 L was distilled off at an atmospheric pressure
8. customto obtain a slurry
9. filtrationThe slurry was filtered
10. customdried