反应详情

温度

180 °C

A solution of 2-[2-(2-chloro-phenoxy)-3-ethoxycarbonyl-allylamino]-5,5,5-trifluoro-pentanoic acid methyl ester (1.43 g, 3.78 mmol) in acetonitrile (4 mL) was placed in a sealed microwave reaction tube and heated in a microwave reactor at 180° C. for 3 h. The mixture was then cooled and concentrated in vacuo with silica gel (3 g). Purification by Biotage flash chromatography (Aspire 40 g column, 16% ethyl acetate/hexanes to 50% ethyl acetate/hexanes) afforded 2-[4-(2-chloro-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-5,5,5-trifluoro-pentanoic acid methyl ester (1.02 g, 50% over two steps) as a an amber oil: HR-ES-MS m/z calculated for C16H15NO4ClF3 [M+H]+ 378.0715, observed 378.0716.

1. temperatureThe mixture was then cooled
2. concentrationconcentrated in vacuo with silica gel (3 g)
3. customPurification by Biotage flash chromatography (Aspire 40 g column, 16% ethyl acetate/hexanes to 50% ethyl acetate/hexanes)