反应详情

温度

90 °C

N,N-Dimethylformamide dimethylacetal (3.9 ml) was added to a solution of ethyl 4-(4-fluorophenyl)-3-oxobutanoate (1310 mg) in n-butyl acetate (15 ml) at room temperature, and the mixture was stirred at 90° C. for five hours. The solvent was distilled off under reduced pressure, and ethanol (20 ml) was added, followed by addition of ethylamine (2 M solution in THF, 4.4 ml). After stirring at 60° C. for two hours, ethylamine (2 M solution in THF, 3.0 ml) was added and the mixture was further stirred at 60° C. for two hours. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography [chloroform:methanol=300:1->70:1 (v/v)] to give 985 mg of the title compound as an oily substance.

1. distillationThe solvent was distilled off under reduced pressure, and ethanol (20 ml)
2. additionwas added
3. additionfollowed by addition of ethylamine (2 M solution in THF, 4.4 ml)
4. stirringAfter stirring at 60° C. for two hours
5. additionethylamine (2 M solution in THF, 3.0 ml) was added
6. stirringthe mixture was further stirred at 60° C. for two hours
7. distillationThe solvent was distilled off under reduced pressure
8. customthe residue was purified by silica gel column chromatography [chloroform:methanol=300:1->70:1 (v/v)]