Reaktion #220198
ord-5f81c07103d8477b9ab602dbda118848
Reaktionsgleichung
Phenyl glyoxal
cyanoacetohydrazide
→
3-Oxo-5-phenyl-2,3-dihydro-pyridazine-4-carbonitrile
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturAfter cooling
- 2Sonstigethe solvent was evaporated
- 3Sonstigethe crude brown mixture was purified by silica chromatography (1:9 methanol/dichloromethane)
- 4SonstigeThe still impure product was further recrystallized from methanol affording 70 mg pure product
Vorschrift
Phenyl glyoxal (1.0 g, 7.46 mmol) and cyanoacetohydrazide (740 mg, 7.46 mmol) were heated to reflux in 10 mL ethanol for 16 hours. After cooling, the solvent was evaporated and the crude brown mixture was purified by silica chromatography (1:9 methanol/dichloromethane). The still impure product was further recrystallized from methanol affording 70 mg pure product.