Hydrazine hydrate (1:1) → HCID 178432964, Verbindung

HRID 1047293Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1047293
O.[NH2:2][NH2:3].[Br:4][C:5]1[CH:6]=[CH:7][C:8]([C:12]#[N:13])=[N:9][C:10]=1[CH3:11]>C(O)C>[Br:4][C:5]1[CH:6]=[CH:7][C:8]([C:12](=[NH:13])[NH:2][NH2:3])=[N:9][C:10]=1[CH3:11]

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 498187795-Bromo-6-methylpyridine-2-carbonitrile

Produkt 1

HCID 178432964HCID 178432964, VerbindungAusbeute 89 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

Hydrazine monohydrate (2 equiv) was added to a stirring 1.2 M suspension of 5-bromo-6-methylpicolinonitrile (1 equiv) in ethanol under nitrogen. The reaction mixture was heated at 50° C. for 24 h. The reaction was cooled to room temperature and then filtered. The collected solid was washed with cold ethanol followed by cold t-butyl methyl ether. The washed solid was dried under vacuum to provide the title compound in 89% yield, as a yellow solid. MS (ESI) m/z 228.9 [M]+, 230.9 [M+2]+.

Aufarbeitung

  1. temperatureThe reaction was cooled to room temperature
  2. filtrationfiltered
  3. washThe collected solid was washed with cold ethanol
  4. customThe washed solid was dried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-6892aeebd47b42418480e075c79c41ed
Quelldatensatz
uspto-grants-2013_10
Patentnummer
US08569494B2

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