3-Nitrophthalic anhydride → 1,4-Phthalazinedione, 2,3-dihydro-5-nitro-

HRID 41964

Reaktionsgleichung

Reaktionsgleichung von HRID 41964
[N+:1]([C:4]1[CH:14]=[CH:13][CH:12]=[C:6]2[C:7]([O:9][C:10](=O)[C:5]=12)=[O:8])([O-:3])=[O:2].O.[NH2:16][NH2:17]>C(O)(=O)C>[N+:1]([C:4]1[CH:14]=[CH:13][CH:12]=[C:6]2[C:5]=1[C:10](=[O:9])[NH:16][NH:17][C:7]2=[O:8])([O-:3])=[O:2]

Komponenten

4

Edukt 2

HCID 216313-Nitrophthalic anhydrideHCID 24654Hydrazine hydrate (1:1)

Produkt 1

HCID 35252231,4-Phthalazinedione, 2,3-dihydro-5-nitro-Ausbeute 92 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

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%.

Aufarbeitung

  1. customA glass flask of the volume 1 l provided with an agitator
  2. additionwas added
  3. filtrationthe crystals of 5-nitro-2,3-dihydrophthalazine-1,4-dione were filtered
  4. washthe sediment was washed on
  5. filtrationa filter with 50 ml of acetic acid and two times with 40 ml of distilled water

Quellen und Nachweise

ORD-Eintrag
ord-9911b083cac04d16b4d8d7c9b4d66c81
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08536171B2

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