反应详情

4-Hydroxybenzaldehyde (15 g, 122 mmol) was dissolved in 150 ml of NMP. 6-Chlorohexanol (20.16 g 146 mmol), anhydrous potassium carbonate (20.36 g, 146 mmol) and a catalytic amount of potassium iodide were added. The batch was stirred at 90 C for 24 hours. Water was added to the cooled solution, which was subsequently extracted with 3×100 mls of ethyl acetate. The combined organics were washed with 5% KOH (2×100 mls), brine solution and then dried over magnesium sulfate. The concentrated product was then recrystallized from a 1:1 mixture of ethyl acetate/hexane to give 14 g of an off-white solid.

1. extractionwas subsequently extracted with 3×100 mls of ethyl acetate
2. washThe combined organics were washed with 5% KOH (2×100 mls), brine solution
3. dry with materialdried over magnesium sulfate
4. customThe concentrated product was then recrystallized from a 1:1 mixture of ethyl acetate/hexane