Hydrazine hydrate (1:1) → 6-Chloro-3-hydrazinyl-4-methylpyridazine

HRID 873969

Reaktionsgleichung

Reaktionsgleichung von HRID 873969
Cl[C:2]1[N:3]=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1[CH3:8].O.[NH2:11][NH2:12]>>[Cl:9][C:5]1[N:4]=[N:3][C:2]([NH:11][NH2:12])=[C:7]([CH3:8])[CH:6]=1

Komponenten

3

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 879233,6-Dichloro-4-methylpyridazine

Produkt 1

HCID 114464906-Chloro-3-hydrazinyl-4-methylpyridazineAusbeute 14,8 %

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A mixture of 3,6-dichloro-4-methylpyridazine (5 g, 30.7 mmol) in hydrazine hydrate (30.4 mL, 153 mmol) was heated up and stirred at 80° C. for 24 hr. The reaction was cooled down to RT; the resulting solid was filtrated off, washed with water and dried under reduced pressure. Recrystallization in hot EtOH followed by trituration in EtOH and ultra sounds afforded the title product (721 mg, 4.55 mmol, 14.8% yield) as white solid. tR: 0.34 min (LC-MS 2); ESI-MS: 159 [M+H]+ (LC-MS 2).

Aufarbeitung

  1. temperaturewas heated up
  2. temperatureThe reaction was cooled down to RT
  3. filtrationthe resulting solid was filtrated off
  4. washwashed with water
  5. customdried under reduced pressure
  6. customRecrystallization in hot EtOH

Quellen und Nachweise

ORD-Eintrag
ord-934d3899d478450293ff5d984e5a67df
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08975417B2

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