反应详情

3750 ml of ethanol and 98.75 grams of potassium hydroxide (1.75 mol) were combined in a 5000 ml three-necked reaction flask, equipped with a magnetic stirrer, a thermometer, a condenser and an addition funnel. After the potassium hydroxide dissolved, 93.75 grams of 4-hydroxybenzoic acid (0.675 mol) and 1.25 grams of potassium iodide were added to the solution. The solution was then heated to reflux, and 81.75 grams of allyl bromide (0.675 mol) was added dropwise to the solution and refluxed overnight. A total of 2000 ml of solvent was then distilled out of the reactor. A layer of solid potassium bromide collected on the internal wall of the flask. The remaining mixture was cooled to room temperature, poured into 2500 ml of water, and neutralized with 6 N aqueous hydrochloric acid. The product precipitated, was filtered, and was washed with deionized water. The crude product was dried under vacuum at 110° C., recrystallized from ethanol (400 ml), and dried again under vacuum, to provide allyloxy benzoic acid.

1. customequipped with a magnetic stirrer
2. temperatureThe solution was then heated
3. temperatureto reflux
4. temperaturerefluxed overnight
5. distillationA total of 2000 ml of solvent was then distilled out of the reactor
6. customA layer of solid potassium bromide collected on the internal wall of the flask
7. additionpoured into 2500 ml of water
8. customThe product precipitated
9. filtrationwas filtered
10. washwas washed with deionized water
11. dry with materialThe crude product was dried under vacuum at 110° C.
12. customrecrystallized from ethanol (400 ml)
13. customdried again under vacuum