Hydrazine hydrate (1:1) → 3-Amino-6-bromopyrazine-2-carbohydrazide

HRID 78726

Reaktionsgleichung

Reaktionsgleichung von HRID 78726
[NH2:1][C:2]1[C:3]([C:9]([O:11]C)=O)=[N:4][C:5]([Br:8])=[CH:6][N:7]=1.O.[NH2:14][NH2:15]>O1CCOCC1>[NH2:1][C:2]1[C:3]([C:9]([NH:14][NH2:15])=[O:11])=[N:4][C:5]([Br:8])=[CH:6][N:7]=1

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 227251Methyl 3-Amino-6-bromopyrazine-2-carboxylate

Produkt 1

HCID 580702563-Amino-6-bromopyrazine-2-carbohydrazide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

Methyl 3-amino-6-bromopyrazine-2-carboxylate (15 g, 64.6 mmol) was suspended in 150 mL of dioxane at room temperature. Hydrazine hydrate (6.5 g, 130 mmol) was added and the reaction mixture was stirred at 60° C. for 2 hours. Initially the mixture became clear, but after a while a precipitate formed. The mixture was cooled to ambient temperature and crude product filtered off. The solid was washed with TBME and subsequently stirred in water. The material was filtered and washed with acetone to afford 3-Amino-6-bromopyrazine-2-carbohydrazide 4 as slightly yellow solid. The material was dried in vacuo. (10.5 g, 70%).

Aufarbeitung

  1. customafter a while a precipitate formed
  2. temperatureThe mixture was cooled to ambient temperature
  3. filtrationcrude product filtered off
  4. washThe solid was washed with TBME
  5. stirringsubsequently stirred in water
  6. filtrationThe material was filtered
  7. washwashed with acetone

Quellen und Nachweise

ORD-Eintrag
ord-be4ae37bcf25498c950d1b45beb2a192
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08841449B2

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