反应详情

温度

90 °C

A reaction mixture containing 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 to the reaction mixture, which was then extracted with toluene. The toluene layer was well washed with water, and then toluene was distilled off. 20 g of sodium hydroxide, 50 mL of water and 200 mL of ethanol were added to the resulting residue, followed by refluxing for 2 hours. Ethanol was distilled off, and hydrochloric acid was added to make the reaction mixture acidic. The mixture was extracted with diethyl ether and dried over anhydrous magnesium sulfate. A residue obtained by distilling the solvent was recrystallized from a mixed solvent of ethanol and water to obtain 29 g of 4-(4-allyloxybutyloxy)benzoic acid.

1. extractionwas then extracted with toluene
2. washThe toluene layer was well washed with water
3. distillationtoluene was distilled off
4. addition20 g of sodium hydroxide, 50 mL of water and 200 mL of ethanol were added to the resulting residue
5. temperatureby refluxing for 2 hours
6. distillationEthanol was distilled off
7. additionhydrochloric acid was added
8. extractionThe mixture was extracted with diethyl ether
9. dry with materialdried over anhydrous magnesium sulfate
10. customA residue obtained
11. distillationby distilling the solvent
12. customwas recrystallized from a mixed solvent of ethanol and water