反应详情

A mixture of 25.0 g of ethyl oxomalonate, 50 ml of isoprene, 80 mg of hydroquinone and 140 ml of acetonitrile were heated for 6 hours under nitrogen in a stainless steel bomb using an oil bath at 135° C. The reaction mixture was cooled overnight and the solvent evaporated. The resulting product was distilled at 120°-130° C. (0.7 mm Hg) to give 29.6 g of an oil, which was flash chromatographed on silica gel using 20% ethyl acetate in hexane as solvent. The resulting fractions 18-40 were evaporated and Kugelrohr distilled to give 26.45 g of the desired product as a mixture of regioisomers.

1. customat 135° C
2. temperatureThe reaction mixture was cooled overnight
3. customthe solvent evaporated
4. distillationThe resulting product was distilled at 120°-130° C. (0.7 mm Hg)