反应详情

温度

90 °C

N,N-Dimethylformamide dimethylacetal (3.6 ml) was added to a solution of ethyl 4-(4-fluorophenyl)-3-oxobutanoate (1200 mg) in n-propyl acetate (13 ml) at room temperature, and the mixture was stirred at 90° C. for four hours. The solvent was distilled off under reduced pressure, and ethanol (18 ml) was added, followed by addition of 2-propylamine (688 μl). After stirring at 60° C. for one hour, 2-propylamine (459 μl) was added and the mixture was further stirred at 60° C. for one hour. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography [chloroform:methanol=300:1->80:1 (v/v)] to give 620 mg of the title compound as an oily substance.

1. distillationThe solvent was distilled off under reduced pressure, and ethanol (18 ml)
2. additionwas added
3. additionfollowed by addition of 2-propylamine (688 μl)
4. stirringAfter stirring at 60° C. for one hour
5. addition2-propylamine (459 μl) was added
6. stirringthe mixture was further stirred at 60° C. for one hour
7. distillationThe solvent was distilled off under reduced pressure
8. customthe residue was purified by silica gel column chromatography [chloroform:methanol=300:1->80:1 (v/v)]