Reaktion #75381

Reaktionsgleichung

4,4-dimethyl-7-acetamino-2H,4H-isoquinoline-1,3-dione

nitric acid

→

4,4-dimethyl-7-acetamino-8-nitro-2H,4H-isoquinoline-1,3-dione

Ausbeute 85.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGThe mixture was stirred for one hour at this temperature
2. 2
   workup.ADDITIONThen, the reaction mixture was poured over ice
3. 3
   Filtrationthe precipitate was suction-filtered off
4. 4
   Waschenwashed neutral with water
5. 5
   Sonstigedried in the air
6. 6
   TemperaturAfter cooling
7. 7
   Filtrationthe crystals were suction-filtered off
8. 8
   Waschenwashed with ether

Vorschrift

220 gm of 4,4-dimethyl-7-acetamino-2H,4H-isoquinoline-1,3-dione were added in portions to 800 ml of fuming nitric acid at -20° C. while stirring. The mixture was stirred for one hour at this temperature. Then, the reaction mixture was poured over ice, the precipitate was suction-filtered off, washed neutral with water, dried in the air, and boiled with isopropanol. After cooling, the crystals were suction-filtered off and washed with ether, yielding 222 gm (85% of theory) of 4,4-dimethyl-7-acetamino-8-nitro-2H,4H-isoquinoline-1,3-dione, m.p. 249° C. (decomp.).

Quelle