Reaktion #73426

Reaktionsgleichung

3-(1-methyl-cyclopropyl)-3-oxo-propionitrile

HCl

methylhydrazine

→

1-Methyl-5-(1-Methyl-cyclopropyl)-1H-pyrazol-3-ylamine

Lösungsmittel

EtOH

Dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenConcentrated under reduced pressure
2. 2
   workup.DISSOLUTIONthe residue is dissolved in MeOH (40 mL)
3. 3
   TemperaturThe mixture is heated at 80° C. for 16 h
4. 4
   EinengenThe solution is then concentrated in vacuo
5. 5
   Sonstigethe residue is purified by HPLC
6. 6
   Sonstigegive product

Vorschrift

To a solution of 3-(1-methyl-cyclopropyl)-3-oxo-propionitrile (1.0 g, 8.1 mmol) in EtOH (10 mL) is added 4N HCl in Dioxane (10 mL). The mixture is stirred at room temperature for 16 hour. Concentrated under reduced pressure, the residue is dissolved in MeOH (40 mL) and treated with methylhydrazine (0.56 g, 12.2 mmol). The mixture is heated at 80° C. for 16 h. The solution is then concentrated in vacuo and the residue is purified by HPLC give product. MS (ESI) m/z 152.3 (M+1).

Quelle