Reaktion #218246

ord-95e62093413b47619e906d83165283e4

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISSOLUTIONdissolved
  2. 2
    workup.ADDITIONThis solution was added
  3. 3
    SonstigeA precipitate formed within 5 minutes
  4. 4
    FiltrationThe precipitate was filtered
  5. 5
    Sonstigeto yield a yellow-orange crystalline solid
  6. 6
    SonstigeThe product was re-crystallized from approximately 30 mL of absolute ethanol

Vorschrift

Concentrated sulfuric acid (2 mL) and 0.4456 g of 2,4-dinitrophenylhydrazine (2,4-DNP) were combined in a 25-mL Erlenmeyer flask. Water was added (2 to 3 mL) dropwise with swirling until the 2,4-DNP dissolved. This was followed by 10 mL of 95% ethanol. This solution was added, dropwise with swirling, to a solution of cyclohexanone, 0.5725 g, dissolved in 20 mL of 95% ethanol. A precipitate formed within 5 minutes. The mixture was refrigerated overnight. The precipitate was filtered to yield a yellow-orange crystalline solid. The product was re-crystallized from approximately 30 mL of absolute ethanol to afford 0.4 g of cyclohexanone 2,4-dinitrophenylhydrazone as orange flakes. The yield was 95%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07384558B2uspto-grants-2008_06