반응 #1532482

ord-f016881d3e9f48bf9d138243e62a3dd7

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07666647B2uspto-grants-2010_02