反应详情

温度

70 °C

A mixture of methyl 2-{(3,4-difluorophenyl)-methylene}-3-oxobutyrate (8.80 g, 36.3 mmol), O-methylisourea hydrogen sulfate (9.40 g, 546 mmol), and NaHCO3 (12.3 g, 146 mol) in DMF (30 mL) was heated at 70° C. with stirring for 16 h. The mixture was cooled, diluted with EtOAc (300 mL) and washed with water (5×300 mL), brine (300 mL), and dried over magnesium sulfate. The solvent was evaporated and the crude product was purified by flash chromatography (EtOAc/hexane, 1/9 to 3/7) as the gradient eluent, giving the desired product as an oil (3.82 g, 35%).

1. temperatureThe mixture was cooled
2. washwashed with water (5×300 mL), brine (300 mL)
3. dry with materialdried over magnesium sulfate
4. customThe solvent was evaporated
5. customthe crude product was purified by flash chromatography (EtOAc/hexane, 1/9 to 3/7) as the gradient eluent