反应详情

温度

150 °C

The following procedure is our modification: A mixture of 5-chloro-6-nitroisoindoline-1,3-dione (28.0 g, 0.123 mol) and urea (73.8 g, 1.23 mol) was stirred at 150° C. for 6 h. Then the temperature was reduced to 90° C., water (400 mL) was added, the mixture was stirred overnight at RT. Precipitate was collected by filtration, water (300 mL) was added and stirred for 4 h at 95° C. The solid was collected by filtration and dried under vacuum. Yellow solid, 19.6 g (94.7 mmol, 77%). LCMS [M−H]− 205.9. 1H NMR (300 MHz, DMSO): δ 11.46 (s, 1H), 8.35 (s, 2H), 8.37 (s, 1H), 7.40 (s, 1H).

1. customwas reduced to 90° C.
2. stirringthe mixture was stirred overnight at RT
3. filtrationPrecipitate was collected by filtration, water (300 mL)
4. additionwas added
5. stirringstirred for 4 h at 95° C
6. filtrationThe solid was collected by filtration
7. customdried under vacuum