Hydrazine hydrate (1:1) → HCID 86650809, Verbindung

HRID 657918Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 657918
[Cl:1][C:2]1[N:3]=[N:4][C:5]([Cl:12])=[CH:6][C:7]=1[C:8]([F:11])([F:10])[F:9].O.[NH2:14][NH2:15]>O1CCOCC1.O.C(#N)C>[ClH:1].[Cl:12][C:5]1[N:4]=[N:3][C:2]([NH:14][NH2:15])=[C:7]([C:8]([F:11])([F:10])[F:9])[CH:6]=1.[ClH:1].[Cl:1][C:2]1[N:3]=[N:4][C:5]([NH:14][NH2:15])=[CH:6][C:7]=1[C:8]([F:11])([F:10])[F:9]

Komponenten

6

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 468472073,6-Dichloro-4-(trifluoromethyl)pyridazine

Produkt 2

HCID 86650809HCID 86650809, VerbindungHCID 86650810HCID 86650810, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 312751,4-DioxaneLösungsmittelHCID 18373917Acetonitrile--water (1/1)Lösungsmittel

Versuchsvorschrift

3,6-Dichloro-4-trifluoromethylpyridazine (W4.004, 150 mg) was dissolved in dioxane (3 ml) and, after hydrazine monohydrate (100 μl) had been added, stirred at RT. After 4 h, the solvent was drawn off and the residue was dissolved in water/ACN and separated by means of preparative HPLC (met. D). The fractions, each of them clean, were combined, freed of the acetonitrile and freeze-dried. 87 mg of (6-chloro-4-trifluoromethylpyridazin-3-yl)hydrazine hydrochloride and 7 mg of (6-chloro-5-trifluoromethylpyridazin-3-yl)hydrazine hydrochloride were obtained.

Aufarbeitung

  1. customseparated by means of preparative HPLC (met. D)
  2. customfreeze-dried

Quellen und Nachweise

ORD-Eintrag
ord-f96fdb6c40c34be1aacc56797c3f4b53
Quelldatensatz
uspto-grants-2011_12
Patentnummer
US08076336B2

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