反应详情

A solution of N-isobutyl-4-oxo-4-phenyl-2-[(trifluoroacetyl)amino]butanamide (0.500 g, 1.45 mmol) and acetic acid (0.831 mL, 14.5 mmol) in toluene (15 mL) was heated to reflux. After 48 hours the reaction was cooled and concentrated. The crude product was purified by chromatography (silica gel, 0 to 50% ethyl acetate in hexane gradient elution) to give the title compound as a solid (0.412 g). MS 327 (M+1) 1H NMR (500 MHz, CDCl3) □ 7.40-7.36 (m, 3H), 7.20 (d, J=2.0 Hz, 1H), 7.12-7.11 (m, 2H), 5.12 (d, J=2.0 Hz, 1H), 3.53 (dd, J=13.9, 9.4 Hz, 1H), 2.61 (dd, J=13.9, 5.9 Hz, 1H), 1.89-1.80 (m, 1H), 0.87 (d, J=6.6 Hz, 3H), 0.84 (d, J=6.6 Hz, 3H).

1. temperatureAfter 48 hours the reaction was cooled
2. concentrationconcentrated
3. customThe crude product was purified by chromatography (silica gel, 0 to 50% ethyl acetate in hexane gradient elution)