反应详情

A solution of 19.85 g (43.4 mmol, purity 81.85%) of diallyl [4-(tert-butoxycarbonyl)benzyl]-malonate, 13.94 g (47.7 mmol, purity 80.5%) of ethyl [1-(2-bromoethyl)cyclopropyl]acetate and 28.56 g (87 mmol) of cesium carbonate in 310 ml of acetonitrile is stirred under reflux for 24 hours. The reaction mixture is then filtered, and the filtrate is concentrated to dryness. The crude product is purified by flash chromatography (3000 g of silica gel 60, mobile phase: cyclohexane/ethyl acetate 20:1). This gives 8 g (35% of theory) of the title compound in the form of a colorless oil.

1. temperatureunder reflux for 24 hours
2. filtrationThe reaction mixture is then filtered
3. concentrationthe filtrate is concentrated to dryness
4. customThe crude product is purified by flash chromatography (3000 g of silica gel 60, mobile phase: cyclohexane/ethyl acetate 20:1)