Reaktion #1999126

ord-57c9c853c6e34252b2b2815618590a54

Lösungsmittel

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas then added
  2. 2
    Einengenethanol was concentrated
  3. 3
    Extraktionfollowed by extraction with ethyl acetate
  4. 4
    WaschenThe extract was washed two or three times with water
  5. 5
    Trocknenthe organic layer was dried over anhydrous MgSO4
  6. 6
    Einengenconcentrated
  7. 7
    SonstigeThe resulting residue was purified by column chromatography (n-hexane:EA=10:1)

Vorschrift

Ethyl 2-benzoylpentanoate (355 mg, 1.5 mmol) was dissolved in 5 mL of ethanol to which 2-hydrazinopyridine (163 mg, 1.5 mmol) was then added, followed by refluxing at 100° C. After 20 hours, ethanol was concentrated, followed by extraction with ethyl acetate. The extract was washed two or three times with water, and the organic layer was dried over anhydrous MgSO4 and then concentrated. The resulting residue was purified by column chromatography (n-hexane:EA=10:1) to afford the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08604210B2uspto-grants-2013_12