反应详情

温度

150 °C

A solution of 3-(2-chloro-phenoxy)-4-(3,3,3-trifluoro-1-methoxycarbonyl-propylamino)-but-2-enoic acid ethyl ester (410 mg, 1.00 mmol) in acetonitrile (4 mL) was placed in a sealed microwave reaction tube and heated in a microwave reactor at 150° C. for 3 h. The mixture was then cooled to room temperature and concentrated in vacuo with silica gel (2 g). Purification by Biotage flash chromatography (Aspire 40 g column, 16% ethyl acetate/hexanes to 33% ethyl acetate/hexanes) afforded 2-[4-(2-chloro-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-4,4,4-trifluoro-butyric acid methyl ester (153 mg, 17% over two steps) as a yellow oil.

1. temperatureThe mixture was then cooled to room temperature
2. concentrationconcentrated in vacuo with silica gel (2 g)
3. customPurification by Biotage flash chromatography (Aspire 40 g column, 16% ethyl acetate/hexanes to 33% ethyl acetate/hexanes)