Reacción #70242

Ecuación de reacción

3-nitrophthalic acid anhydride

hydrazine hydrate

→

5-Nitro-2,3-Dihydrophthalazine-1,4-Dione

Rendimiento 92.0%

Disolventes

acetic acid

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroA glass flask of the volume 1 l provided with an agitator
2. 2
   workup.ADDITIONwas added
3. 3
   Filtraciónthe crystals of 5-nitro-2,3-dihydrophthalazine-1,4-dione were filtered
4. 4
   Lavadothe sediment was washed on
5. 5
   Filtracióna filter with 50 ml of acetic acid and two times with 40 ml of distilled water

Procedimiento

A glass flask of the volume 1 l provided with an agitator, a thermometer, a condenser and a capillary was filled with 600 ml of icy acetic acid and 154.5 g (0.8 mole) of 3-nitrophthalic acid anhydride, thereafter it was heated to the temperature of 110° C. and gradually 44.1 g (0.88 mole) of hydrazine hydrate was added. Next the reaction mixture was kept at the state of boiling for 30 minutes thereafter it was cooled to the temperature of 80° C., the crystals of 5-nitro-2,3-dihydrophthalazine-1,4-dione were filtered, the sediment was washed on a filter with 50 ml of acetic acid and two times with 40 ml of distilled water. The total amount of 5-nitro-2,3-dihydrophthalazine-1,4-dione was 228.7 g, the yield was 92%.

Fuente