Reaktion #1828437

ord-5616ef379a354c0facc65c10679039f9

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was then removed from the mixture
  2. 2
    workup.ADDITION200 mL of water was added to the residue and mixture
  3. 3
    workup.ADDITIONwas neutralized by the addition of solid NaHCO3
  4. 4
    ExtraktionThe product was extracted into ether
  5. 5
    ExtraktionThe ether extract
  6. 6
    Trocknenwas dried over Na2SO4
  7. 7
    Sonstigeevaporated
  8. 8
    Sonstigeto give 5.8 g as an oil which
  9. 9
    Sonstigewas used in the next reaction without farther purification

Vorschrift

A mixture of ethyl 3-ethyl-2,4-dioxo-4-(2,4,6trimethylphenyl)butanoate (6.0 g, 20.7 mmol) and hydrazine dihydrochloride (2.17 g, 20.7 mmoL) in 100 mL of EtOH was stirred at 80° C. for 6 hours. The solvent was then removed from the mixture. 200 mL of water was added to the residue and mixture was neutralized by the addition of solid NaHCO3. The product was extracted into ether. The ether extract was dried over Na2SO4 and evaporated to give 5.8 g as an oil which was used in the next reaction without farther purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05973152uspto-grants-1999_10