反应详情

A mixture of 4-hydroxyphenylpropan-2-one ethylene ketal (3.0 g) and potassium carbonate (2.13 g) in acetone (50 ml) was treated with methyl 4-bromocrotonate (2.77 g) and a trace of potassium iodide. After heating under reflux for 12 hours, the solution was filtered, the solvent evaporated and the residue dissolved in methanol (50 ml) and 2.5 N hydrochloric acid (25 ml). The solution was stirred at ambient temperature for 2 hours, the solvent evaporated, the residue extracted with ether, washed with 2 N sodium hydroxide, water and dried (MgSO4). Removal of the solvent gave the title compound as an oil (2.3 g).

1. temperatureAfter heating
2. temperatureunder reflux for 12 hours
3. filtrationthe solution was filtered
4. customthe solvent evaporated
5. dissolutionthe residue dissolved in methanol (50 ml)
6. customthe solvent evaporated
7. extractionthe residue extracted with ether
8. washwashed with 2 N sodium hydroxide, water
9. dry with materialdried (MgSO4)
10. customRemoval of the solvent