反应详情

温度

125 °C

1-(4-Chloro-phenyl)-propan-2-one (8.6 g, 51 mmol) and Eschenmoser's salt (12.3 g, 66.3 mmol) were dissolved in glacial acetic acid and heated in a closed pressure tube at 125° C. under nitrogen for 1 h. After cooling to room temperature, the solution was concentrated. The residue was dissolved in EtOAc, washed with saturated NaHCO3 aqueous solution, dried (MgSO4), concentrated, and chromatographed (SiO2, 39:1-19:1 hexane/EtOAc) to give 3-(4-chloro-phenyl)-but-3-en-2-one as yellow oil (3.92 g, 43%).

1. temperatureAfter cooling to room temperature
2. concentrationthe solution was concentrated
3. dissolutionThe residue was dissolved in EtOAc
4. washwashed with saturated NaHCO3 aqueous solution
5. dry with materialdried (MgSO4)
6. concentrationconcentrated
7. customchromatographed (SiO2, 39:1-19:1 hexane/EtOAc)