Hydrazine → HCID 58772592, Verbindung
Reaktionsgleichung
[NH2:1][NH2:2].[Cl:3][C:4]1[N:5]=[N:6][C:7](Cl)=[CH:8][C:9]=1[C:10]1[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][CH:11]=1>N1C=CC=CC=1>[Cl:3][C:4]1[N:5]=[N:6][C:7]([NH:1][NH2:2])=[CH:8][C:9]=1[C:10]1[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][CH:11]=1Komponenten
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 100 °C
Versuchsvorschrift
Anhydrous hydrazine (8 mL) was added to a solution of 3,6-dichloro-4-(4-chlorophenyl)pyridazine (7.1 g, 27.4 mmol) in pyridine (30 mL) at 100° C. The resulting mixture was stirred at 100° C. for 30 min. Analysis by HPLC/MS indicated the reaction was complete. After cooling to room temperature, the reaction mixture was concentrated under reduced pressure to remove most of the pyridine. To the residue was added isopropanol (200 mL), the resulting suspension was refluxed for 20 min. After cooling to room temperature, the suspension was filtered. The collected solid was washed with isopropanol, dried in a 50° C. vacuum oven overnight to afford 4.0 g (57%) of the title compound as an off-white solid. LC/MS (method A): retention time=2.24 min, (M+H)+=255.
Aufarbeitung
- temperatureAfter cooling to room temperature
- concentrationthe reaction mixture was concentrated under reduced pressure
- customto remove most of the pyridine
- additionTo the residue was added isopropanol (200 mL)
- temperaturethe resulting suspension was refluxed for 20 min
- temperatureAfter cooling to room temperature
- filtrationthe suspension was filtered
- washThe collected solid was washed with isopropanol
- customdried in a 50° C. vacuum oven overnight
Quellen und Nachweise
- ORD-Eintrag
- ord-2920fb589f9441aca1570fa6d3f0c11a
- Quelldatensatz
- uspto-grants-2008_01
- Patentnummer
- US07317012B2
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