Methanesulfonic Acid → HCID 23293363, compound

Participants

Reaction Steps

4-Hydroxyacetophenone (75.00 g, 0.55 mol) was dissolved in ethyl acetate (300 ml) and a catalytic amount of methanesulfonic acid. The solution was cooled to 0°-4° C. Dihydropyran (204 ml, 2.20 moles, 4.0 eq) was slowly added. At the end of the addition, the ice-water bath was removed and the reaction was allowed to proceed at room temperature. A few minutes later a heavy white precipitate was formed and the slurry was transferred into a separatory funnel where it was washed with water. The organic layer was dried over anhydrous sodium sulfate. Removal of the solvent under reduced pressure afforded a white fluffy solid. The solid was recrystallized from hexane. The yield was quantitative.

Provenance & Evidence