反应详情

A solution of 8.9 parts of intermediate 13, namely 5-benzoyl-2-nitrobenzonitrile, 166 parts of sulfuric acid and 10 parts of water was heated at 90° C. for 13/4 hours. The reaction mixture was poured into ice-water. The precipitate was filtered off and recrystallized from methanol. The product was filtered off, washed with methanol and 2,2'-oxybispropane and dried in vacuo at 60°-70° C., yielding 5.23 parts (54.8%) of 5-benzoyl-2-nitrobenzamide; mp. 244.3° C. (intermediate 14).

1. filtrationThe precipitate was filtered off
2. customrecrystallized from methanol
3. filtrationThe product was filtered off
4. washwashed with methanol and 2,2'-oxybispropane
5. customdried in vacuo at 60°-70° C.