反应详情

温度

90 °C

A solution comprising 14 g of allyl (4-chlorobutyl ether, 14 g of 4-hydroxybenzoic acid, 14 g of potassium carbonate and 50 ml of dimethylformamide was stirred at 90° C. for 3 hours. Water was added thereto, and the liquid was extracted with toluene. The toluene layer was washed well with water, and toluene was distilled off. Sodium hydroxide 20 g, water 50 ml and ethanol 200 ml were added to the resulting residue, and the solution was refluxed for 2 hours. Ethanol was distilled off, and hydrochloric acid was added to acidify the solution. It was extracted with diethyl ether and dried on anhydrous magnesium sulfate. The solvent was distilled off, and a residue thus obtained was recrystallized from a mixed solvent of ethanol and water to obtain 29 g of 4-(4-allyloxybutyloxy)benzoic acid. Phase transition temperature: C 94 N 107 I

1. extractionthe liquid was extracted with toluene
2. washThe toluene layer was washed well with water, and toluene
3. distillationwas distilled off
4. additionSodium hydroxide 20 g, water 50 ml and ethanol 200 ml were added to the resulting residue
5. temperaturethe solution was refluxed for 2 hours
6. distillationEthanol was distilled off
7. additionhydrochloric acid was added
8. extractionIt was extracted with diethyl ether
9. dry with materialdried on anhydrous magnesium sulfate
10. distillationThe solvent was distilled off
11. customa residue thus obtained
12. customwas recrystallized from a mixed solvent of ethanol and water