反应详情

温度

100 °C

Aniline derivative 16 (0.89 g, 5.0 mmol) was dissolved in pyridine (25 mL). Succinic anhydride (0.75 g, 7.5 mmol) was added together with 4-N,N,-dimethylaminopyridine (63 mg, 0.5 mmol) and the mixture was stirred overnight at 100° C. The solution was concentrated under reduced pressure and the pale brown solid was recrystallized from a mixture of EtOH/MeOH/H2O (60 mL, 5/35/1, v/v/v). After filtration, the mother liquid was concentrated to ˜10 mL to give carboxylic acid 17 as a solid which was dried under vacuum at 50° C. for 16 h. Yield 1.28 g (92%). Rf 0.3 (DCM/MeOH/AcOH, 100/10/1, v/v/v).

1. concentrationThe solution was concentrated under reduced pressure
2. customthe pale brown solid was recrystallized from a mixture of EtOH/MeOH/H2O (60 mL, 5/35/1, v/v/v)
3. filtrationAfter filtration
4. concentrationthe mother liquid was concentrated to ˜10 mL