反应详情

温度

-78 °C

8-Chloro-3-methoxy-2,5-dioxo-2,5-dihydro-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 26° C. for 22.5 hours. The excess ammonia was evaporated to give a solid. The solid was recrystallized from 5 mL hot dimethylformamide and water; crystallization was initiated by cooling the solution in an ice bath. The solid was filtered, washed (water) and vacuum dried (100° C., 15 Pa) to give the title compound (0.274 g); mp 344.5°-346.4° C. (dec); NMR: 11.47 (s,1), 8.10 (d,1, J=8.7), 7.53 (d,1, J=2.0), 7.27 (dd,1, J=8.7, 2.0), 7.1 (broad s,2, NH2), 6.23 (s,1).

1. customThe mixture was sealed in a pressure vessel
2. temperaturewarmed to 26° C. for 22.5 hours
3. customThe excess ammonia was evaporated
4. customto give a solid
5. customThe solid was recrystallized from 5 mL hot dimethylformamide and water
6. customcrystallization
7. temperatureby cooling the solution in an ice bath
8. filtrationThe solid was filtered
9. washwashed (water) and vacuum
10. customdried (100° C., 15 Pa)