反应详情

A pressure reactor was charged with 2-methyl-4-nitro-1H-isoindole-1,3(2H)-dione (59.0 g, 0.286 mol), 1 L acetic acid, and 2 q 5% Pd/C. The reactor was pressurized to 48 psi hydrogen, and the exothermic reaction was complete in 2 hours. The catalyst was removed with hot filtration, and the filtrate combined with the contents of another reactor which contained 53.2 g of 3-nitrophthalimide under the same conditions. The acetic acid was removed at the rotovap, then the salt was cracked by adding 2 M ammonium hydroxide. The slurry was stirred 30 minutes; then filtered; washed with water, ethanol, and ether; and dried at the pump to give 91.4 g, 95% of the product.

1. customthe exothermic reaction
2. customThe catalyst was removed with hot filtration
3. customthe filtrate combined with the contents of another reactor
4. customThe acetic acid was removed at the rotovap
5. additionby adding 2 M ammonium hydroxide
6. filtrationthen filtered
7. washwashed with water, ethanol, and ether
8. customand dried at the pump