反应详情

A mixture of 3-(4-bromo-phenyl)-3-(4-chloro-phenyl)-2-cyano-propionic acid ethyl ester (1.91, 4.87 mmol), acetic acid (10 ml), concentrated sulfuric acid (5 ml) and water (5 ml) were refluxed for 2 hours. Reaction mixture was poured into iced water and extracted with ethyl acetate. The organic layer was separated, dried (MgSO4), filtered and concentrated, the crude product was purified over flash silica chromatography eluting with ethyl acetate/petroleum ether (1:1) to afford the desired product (0.82 g, 50% yield). LC/MS: (PS-A2) Rt 3.39 [M+H]− 338.86.

1. temperaturewere refluxed for 2 hours
2. customReaction mixture
3. extractionextracted with ethyl acetate
4. customThe organic layer was separated
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated
8. customthe crude product was purified over flash silica chromatography
9. washeluting with ethyl acetate/petroleum ether (1:1)