Hydrazine hydrate (1:1) → HCID 55285667, Verbindung

HRID 1943931Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1943931
[CH:1]([NH:4]/[C:5](/SC)=[CH:6]/[C:7]#[N:8])([CH3:3])[CH3:2].O.[NH2:12][NH2:13]>CCO>[CH:1]([NH:4][C:5]1[CH:6]=[C:7]([NH2:8])[NH:13][N:12]=1)([CH3:3])[CH3:2]

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 86652503(2Z)-3-[(1-Methylethyl)amino]-3-(methylthio)-2-propenenitrile

Produkt 1

HCID 55285667HCID 55285667, VerbindungAusbeute 62,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of (Z)-3-(isopropylamino)-3-(methylthio)acrylonitrile (0.413 g, 2.64 mmol) and hydrazine monohydrate (0.38 mL, 7.93 mmol) in EtOH (6 mL) was heated to reflux for 16 hours. After cooling to room temperature, the reaction mixture was concentrated. The residue was purified by column chromatography, eluting with ethyl acetate, DCM/MeOH (9:1) to give N3-isopropyl-1H-pyrazole-3,5-diamine (0.231 g, 62% over 2 steps) as an oil.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureto reflux for 16 hours
  3. concentrationthe reaction mixture was concentrated
  4. customThe residue was purified by column chromatography
  5. washeluting with ethyl acetate, DCM/MeOH (9:1)

Quellen und Nachweise

ORD-Eintrag
ord-1aa0d19f5a26406592838b4bfdc8bdfc
Quelldatensatz
uspto-grants-2013_03
Patentnummer
US08394795B2

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