Water → Luminol

HRID 2296623Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2296623
[Na].NC1C=CC=C2C=1C(=O)[NH:6][NH:7]C2=[O:13].O.NN.[N+:18]([C:21]1[CH:30]=[CH:29][CH:28]=[C:27]2[C:22]=1[C:23](=[O:32])[NH:24][NH:25][C:26]2=[O:31])([O-])=O.O>[Ni].C(O)(=O)C>[OH2:13].[NH2:6][NH2:7].[NH2:18][C:21]1[CH:30]=[CH:29][CH:28]=[C:27]2[C:22]=1[C:23](=[O:32])[NH:24][NH:25][C:26]2=[O:31]

Komponenten

8

Edukt 4

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)2×HCID 35252231,4-Phthalazinedione, 2,3-dihydro-5-nitro-HCID 9794222Luminol sodium salt

Produkt 2

HCID 10638LuminolHCID 24654Hydrazine hydrate (1:1)

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 935NickelKatalysator2×HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

This problem was solved by a method for manufacturing 5-amino-2,3-dihydrophthalazine-1,4-dione sodium salt, comprising reduction of the product by hydrazine hydrate in presence of a skeletal nickel catalyst, first by interacting 3-nitro-phthalanhydride with hydrazine hydrate in acetic acid at 90-120° C. with formation of 5-nitro-2,3-dihydrophthalazine-1,4-dione, after reduction thereof by hydrazine hydrate in a water-alkaline medium in presence of a skeletal nickel catalyst, isolating 5-amino-2,3-dihydrophthalazine-1,4-dione, which is then treated by sodium hydroxide in the presence of a lower alcohol or a ketone at 20-80° C. to obtain the target product.

Aufarbeitung

  1. customat 90-120° C.

Quellen und Nachweise

ORD-Eintrag
ord-fe43f75a723949d6b88c3bf6b625f220
Quelldatensatz
uspto-grants-2002_12
Patentnummer
US06489326B1

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