Reaktion #62284

Reaktionsgleichung

α-cyanoacetophenone

benzyl hydrazine dihydrochloride

triethylamine

→

title compound

Ausbeute 82.3%

2-Benzyl-5-phenyl-2H-pyrazol-3-ylamine

Ausbeute 82.3%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated
2. 2
   Temperaturunder reflux for 4 hours
3. 3
   SonstigeThe solvent was evaporated
4. 4
   workup.ADDITIONthe residue was added with water
5. 5
   Extraktionextracted with ethyl acetate
6. 6
   Trocknendried over anhydrous sodium sulfate
7. 7
   workup.DISTILLATIONAfter distilling off the solvent
8. 8
   Sonstigethe residue was purified
9. 9
   Sonstigeseparated by silica gel column chromatography (ethyl acetate:n-hexane=1:4)

Vorschrift

2.9 g of α-cyanoacetophenone and 3.9 g of benzyl hydrazine dihydrochloride were suspended in 50 mL of ethanol. The reaction solution was added with 6.0 ml of triethylamine at room temperature, and heated under reflux for 4 hours. The solvent was evaporated, and the residue was added with water, extracted with ethyl acetate, and dried over anhydrous sodium sulfate. After distilling off the solvent, the residue was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:4), to afford 4.1 g of the title compound as a yellow needle powder.

Quelle