Hydrochloric Acid → HCID 21081843, Verbindung

HRID 346511

Reaktionsgleichung

Reaktionsgleichung von HRID 346511
[NH:1]([C:3]1[N:8]=[N:7][C:6]([N:9]([CH3:16])[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:5][CH:4]=1)[NH2:2].[Cl:17][C:18]1[N:23]=[C:22]([C:24](O)=[O:25])[CH:21]=[CH:20][CH:19]=1.Cl>C(Cl)Cl>[Cl:17][C:18]1[N:23]=[C:22]([C:24]([NH:2][NH:1][C:3]2[N:8]=[N:7][C:6]([N:9]([CH3:16])[C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=3)=[CH:5][CH:4]=2)=[O:25])[CH:21]=[CH:20][CH:19]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 208126-Chloropicolinic acidHCID 210818446-Hydrazinyl-N-methyl-N-phenyl-3-pyridazinamine

Produkt 1

HCID 21081843HCID 21081843, VerbindungAusbeute 30,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 6-hydrazino-N-methyl-N-phenylpyridazine-3-amine (1.14 g) in methylene chloride (10 ml), 6-chloropicolic acid (0.83 g) and WSCD hydrochloride (1.22 g) were added, and the mixture was stirred at room temperature overnight. The reaction solution was purified by silica gel column chromatography (eluent: chloroform) to obtain 6-chloro-N′-{6-[methyl(phenyl)amino]pyridazin-3-yl}pyridine-2-carbohydrazide (0.57 g). This compound (0.56 g) was stirred at 150° C. overnight in xylene (20 ml), and the reaction solution was concentrated to obtain 3-(chloropyridin-2-yl)-N-methyl-N-phenyl-1,2,4-triazolo[4,3-b]pyridazine-6-amine (0.54 g) as colorless solids.

Aufarbeitung

  1. customThe reaction solution was purified by silica gel column chromatography (eluent: chloroform)

Quellen und Nachweise

ORD-Eintrag
ord-0d15d04f87134a0ea1bdf49eb3d5b4f2
Quelldatensatz
uspto-grants-2007_02
Patentnummer
US07173033B2

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