Ethanol → HCID 86747927, compound

Participants

Reaction Steps

A mixture was prepared from 25% aqueous hydroxylammonium sulfate (39.0 g, 0.060 mol) and 50% aqueous sodium hydroxide (9.6 g, 0.12 mol). 40 mL of ethanol was then added and the mixture was allowed to cool to room temperature and filtered to remove sodium sulfate. The filtered solution was placed in a 250-mL, 3-necked flask equipped with a reflux condenser, thermometer, heating mantle, stirrer, pH electrode, and dropping funnel. Then an α,β-unsaturated ester (ethyl crotonate or ethyl acrylate) (0.10 mole) was added and the mixture was stirred at room temperature for 60 minutes. Then an α,β-unsaturated carbonyl compound (0.125 mole) was added all at once. About 10 mL of acetic acid was added to lower the pH to below 4.0 and the reaction mixture was heated to reflux for 3 to 5 hours.

Provenance & Evidence