Water → 6-Chloro-3-hydrazinyl-4-methylpyridazine

HRID 874013

Reaktionsgleichung

Reaktionsgleichung von HRID 874013
Cl[C:2]1[N:3]=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1[CH3:8].O.[NH2:11][NH2:12].O>CCO>[Cl:9][C:5]1[N:4]=[N:3][C:2]([NH:11][NH2:12])=[C:7]([CH3:8])[CH:6]=1

Komponenten

5

Edukt 3

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 879233,6-Dichloro-4-methylpyridazine

Produkt 1

HCID 114464906-Chloro-3-hydrazinyl-4-methylpyridazineAusbeute 39,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

3,6-Dichloro-4-methylpyridazine (Combi-Blocks) (60 g, 361 mmol) was dissolved in hydrazine monohydrate (Aldrich) (335 mL, 5411 mmol) and the solution was stirred at 80° C. for 1 h, forming a white precipitate. The reaction mixture is dilutes with water and the precipitated products isolated by filtration. The solid crude product is suspended in EtOH and left in an ultra sound bath for 1 h. The desired product (22.4 g) was obtained after filtration and drying under vacuum as a beige solid. tR: 0.31 min (LC-MS 2); ESI-MS: 160.0 [M+H]+ (LC-MS 2). 1H NMR (400 MHz; DMSO-d6) δ ppm 7.83 (br.s, 1H) 7.32 (s, 1H) 4.49 (br.s, 2H) 2.05 (s, 3H).

Aufarbeitung

  1. customforming a white precipitate
  2. customthe precipitated products isolated by filtration
  3. waitleft in an ultra sound bath for 1 h

Quellen und Nachweise

ORD-Eintrag
ord-cb3edca2b4dd4f3fab854d9cc4acc786
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08975417B2

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