反应详情

77.5 g (0.22 mol) of 4-Octyloxy-2-(pent-4-en-1-yloxy)benzoic acid methyl ester obtained in Step 2 is dissolved in 700 mL of THF. A solution of 66.6 (1.19 mol) of KOH in 200 mL of water is added. The mixture is heated to reflux and stirred for 6 h. The mixture is allowed to return to room temperature, then the solvents are distilled off and ice/water is added. After acidification with concentrated HCl, the mixture is extracted with several times with CH2Cl2. The resulting organic phase is dried over magnesium sulfate and concentrated under reduced pressure. The product recrystallised from hexane gives a pure product as white crystals (66.9 g, 92%).

1. temperatureThe mixture is heated
2. temperatureto reflux
3. customto return to room temperature
4. distillationthe solvents are distilled off
5. additionice/water is added
6. extractionAfter acidification with concentrated HCl, the mixture is extracted with several times with CH2Cl2
7. dry with materialThe resulting organic phase is dried over magnesium sulfate
8. concentrationconcentrated under reduced pressure
9. customThe product recrystallised from hexane