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

HRID 380322

Reaktionsgleichung

Reaktionsgleichung von HRID 380322
[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 (22.5 g, 0.11 mol) and hydrazine hydrate (34 ml, 0.66 mol) were heated at reflux in dioxane (280 ml) for 24 hours. Upon cooling the desired isomer crystallized from the reaction and was collected by filtration (13.3 g, 64%). 1H NMR (250 MHz , d6-DMSO) 1.68-1.86 (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 (13.3 g, 64%)

Quellen und Nachweise

ORD-Eintrag
ord-ee749b0974f94195a9d027d4446f3588
Quelldatensatz
uspto-grants-2001_10
Patentnummer
US06303605B1

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