反应详情

温度

-78 °C

2,5-Dihydro-2,5-dioxo-3-methoxy-1H-benz[b]azepine (0.4 g) was treated with 80 mL of liquid anhydrous ammonia chilled to -78° C. The mixture was sealed in a pressure vessel and warmed to 23° C. for 18 hours. The excess ammonia was evaporated to give a solid. The solid was dissolved in hot methanol (120 mL); the solution was filtered and evaporated to 60 mL; and crystallization was initiated by cooling the solution in an ice bath. The solid was filtered, washed (cold methanol) and dried under vacuum (25° C., 15 Pa) to give the title compound (0.28 g); mp 295.2-296.5° C. (dec); NMR: 11.38 )s,1, NH), 8.09 dd,1, J=8.2, 1.6), 7.54 (m,1), 7.44 (dd,1, J=8.2, 1.6), 7.21 (m,1), 6.23 (s,1). Analysis for C10H8N2O2 : Calculated: C, 63.82; H, 4.28; N, 14.89; Found: C, 63.80; H, 4.41; N, 14.87.

1. customThe mixture was sealed in a pressure vessel
2. temperaturewarmed to 23° C. for 18 hours
3. customThe excess ammonia was evaporated
4. customto give a solid
5. filtrationthe solution was filtered
6. customevaporated to 60 mL
7. customand crystallization
8. temperatureby cooling the solution in an ice bath
9. filtrationThe solid was filtered
10. washwashed (cold methanol)
11. customdried under vacuum (25° C., 15 Pa)