Reacción #220198

ord-5f81c07103d8477b9ab602dbda118848

Reactivos

Ninguno

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaAfter cooling
  2. 2
    Otrothe solvent was evaporated
  3. 3
    Otrothe crude brown mixture was purified by silica chromatography (1:9 methanol/dichloromethane)
  4. 4
    OtroThe still impure product was further recrystallized from methanol affording 70 mg pure product

Procedimiento

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.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07390808B2uspto-grants-2008_06