反应详情

A mixture of 8.54 g (0.035 mole) of 4-amino-3-iodobenzonitrile (31), 16 mL (16.32 g, 0.16 mole) of acetic anhydride and five drops of concentrated sulfuric acid was heated at 70° under reflux for 10 minutes (the mixture became thick when the temperature reached 40° and some manual stirring was required). The reaction mixture was poured over 400 mL of cold water and stirred for 5 minutes to give a white solid which was filtered and dried, yielding 9.48 g (95%) of 32 as white powder, mp 176-181°. Infrared (IR) and NMR analysis gave the following results:

1. temperaturewas heated at 70°
2. temperatureunder reflux for 10 minutes (the mixture
3. customreached 40°
4. stirringstirred for 5 minutes
5. customto give a white solid which
6. filtrationwas filtered
7. customdried