反应详情

温度

40 °C

A 3-L flask equipped with a stirrer, cooling tube and thermometer was purged by nitrogen gas. 55.2 g (770 mmol) of hydroxylamine-hydrochloride (purity of 97%) and 1.2 L of pyridine were added to the flask and were stirred to dissolve at room temperature under nitrogen atmosphere. To the stirred mixture, 138.7 g (700 mmol) of 1,8-naphthalenedicarboxylic anhydride was added. The stirred mixture was heated at 40° C. for 1 hour and subsequently was heated at 70° C. for 1 hour. After stirring at 90° C. for 1 hour, the reaction mixture was cooled to room temperature with stirring. The resulting crystalline solid was filtered off and washed with 5% by weight of acetic acid aqueous solution and dried at 80° C. for 20 hours under a reduced pressure to yield 120.7 g (81%) of N-hydroxynaphthalimide with yellow color.

1. customA 3-L flask equipped with a stirrer
2. temperaturecooling tube
3. customthermometer was purged by nitrogen gas
4. dissolutionto dissolve at room temperature under nitrogen atmosphere
5. temperaturesubsequently was heated at 70° C. for 1 hour
6. stirringAfter stirring at 90° C. for 1 hour
7. temperaturethe reaction mixture was cooled to room temperature
8. stirringwith stirring
9. filtrationThe resulting crystalline solid was filtered off
10. washwashed with 5% by weight of acetic acid aqueous solution
11. customdried at 80° C. for 20 hours under a reduced pressure