Hydrazine hydrate (1:1) → 3-chloro-4-cyclobutyl-6-hydrazinylPyridazine

HRID 1369419Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1369419
[Cl:1][C:2]1[N:3]=[N:4][C:5](Cl)=[CH:6][C:7]=1[CH:8]1[CH2:11][CH2:10][CH2:9]1.O.[NH2:14][NH2:15]>O1CCOCC1>[Cl:1][C:2]1[N:3]=[N:4][C:5]([NH:14][NH2:15])=[CH:6][C:7]=1[CH:8]1[CH2:11][CH2:10][CH2:9]1

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 219732193,6-Dichloro-4-cyclobutylpyridazine

Produkt 1

HCID 226099463-chloro-4-cyclobutyl-6-hydrazinylPyridazine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

3,6-Dichloro-4-cyclobutylpyridazine (10 g, 0.049 mol) and hydrazine hydrate (14 ml, 0.30 mol) were heated at reflux in dioxan (125 ml) for 24 hours. Upon cooling the desired isomer crystallized from the reaction and was collected by filtration (4.8 g, 49%). 1H NMR (250 MHz, d6-DMSO) δ1.68-1.86 (1H, m), 2.00-2.11 (3H, m), 2.29-2.38 (2H, m), 3.52-3.61 (1H, m) 4,35 (2H, br), 6.99 (1H, s), 8.06 (1H, br); MS (ES+) m/e 198 [MH]+, 200 [MH]+.

Aufarbeitung

  1. temperatureUpon cooling the desired isomer
  2. customcrystallized from the reaction
  3. filtrationwas collected by filtration (4.8 g, 49%)

Quellen und Nachweise

ORD-Eintrag
ord-3dcea6574ce2453d9c9552b395ff1f69
Quelldatensatz
uspto-grants-2003_06
Patentnummer
US06579875B1

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