Reaktion #1532482

ord-f016881d3e9f48bf9d138243e62a3dd7

Reaktionsgleichung

O=CC(=O)c1ccccc1
Phenyl glyoxal
N#CCC(=O)NN
cyanoacetohydrazide
N#Cc1c(-c2ccccc2)cn[nH]c1=O
3-Oxo-5-phenyl-2,3-dihydro-pyridazine-4-carbonitrile

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling
  2. 2
    Sonstigethe solvent was evaporated
  3. 3
    Sonstigethe crude brown mixture was purified by silica chromatography (1:9 methanol/dichloromethane)
  4. 4
    SonstigeThe 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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07666647B2uspto-grants-2010_02