反应详情

温度

140 °C

A suspension of 3-oxo-3-{[3-(trifluoromethyl)phenyl]amino}propanoic acid (3.26 g; 13.0 mmol; 1 eq) in polyphosphoric acid (26.4 g) is allowed to stir for 4 hours at 140° C. The mixture becomes limpid after 1 h30 stirring. After cooling to room temperature, the orange solution is taken-up in water (100 mL) and sonicated for 5 minutes. The resulting fine powder is filtrated and washed with cold water (4×20 mL). The solid is taken up several times in ethanol (3×100 mL) and concentrated to afford the title compound as a dry light orange powder (2.19 g; 9.6 mmol; 74%).

1. temperatureAfter cooling to room temperature
2. customsonicated for 5 minutes
3. filtrationThe resulting fine powder is filtrated
4. washwashed with cold water (4×20 mL)
5. concentrationconcentrated