反应详情

温度

120 °C

p-Anisidine (29 mg, 0.24 mmol) was dissolved in toluene (2 ml) in a reaction vessel, and trimethylaluminum (2 M in TIIF, 0.12 ml) was added thereto at 0° C. After stirring for 10 min, to the mixture was added methyl 3-amino-4-phenylthiophene-2-carboxylate (50 mg, 0.21 mmol). The resulting mixture was heated to reflux at 120° C. for 16 hr. The completion of the reaction was confirmed by TLC. The reaction mixture was allowed to cool to room temperature, extracted with EtOAc, dried over anhydrous MgSO4, and concentrated under reduced pressure. The concentrate was purified by silica gel column chromatography (hexane:EtOAc=5:1) to give (57 mg, 0.18 mmol, 84% yield) of the title compound.

1. customat 0° C
2. temperatureThe resulting mixture was heated
3. temperatureto cool to room temperature
4. extractionextracted with EtOAc
5. dry with materialdried over anhydrous MgSO4
6. concentrationconcentrated under reduced pressure
7. customThe concentrate was purified by silica gel column chromatography (hexane:EtOAc=5:1)