反应详情

温度

100 °C

A mixture of valeric acid (5.50 mL, 50.4 mmol), 2,3-diaminopyridine (5.0 g, 45.8 mmol), and polyphosphoric acid (50 g) was heated to 100° C. with stirring for 5 hours. Basification (NH4OH), extraction (EtOAc, 4×20 mL), drying (K2CO3), and concentration gave 7.61 g (95%) of the title compound as an amorphous tan solid which was judged pure by 1H NMR and tlc (mp ca 80° C. without recrystallization).

1. extractionBasification (NH4OH), extraction (EtOAc, 4×20 mL)
2. customdrying
3. concentration(K2CO3), and concentration