Reaktion #960692

ord-edd513daf82746358a670343f1f156b9

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto react at room temperature for 5 hours
  2. 2
    Sonstigereaction solution
  3. 3
    Sonstigethe resultant reaction solution
  4. 4
    Extraktionwas extracted with ethyl acetate
  5. 5
    WaschenThe organic layer was washed with saturated brine
  6. 6
    Trocknendried over anhydrous sodium sulfate
  7. 7
    workup.DISTILLATIONThe solvent was distilled off
  8. 8
    Sonstigethe residue was purified with the use of a silica gel column
  9. 9
    SonstigeIn this way, Compound V-1 was obtained

Vorschrift

Tetrahydrofuran (0.72 ml), a 37% formaldehyde aqueous solution (0.242 ml), and potassium carbonate (0.50 mmol) were added to 1-(4-chlorobenzyl)-2-oxocyclopentanecarboxylic acid methyl ester (Compound VI-1) (1.0 mmol), and the mixture was allowed to react at room temperature for 5 hours. Water was added to the resultant reaction solution, and the resultant reaction solution was extracted with ethyl acetate. The organic layer was washed with saturated brine, and thereafter dried over anhydrous sodium sulfate. The solvent was distilled off, and the residue was purified with the use of a silica gel column. In this way, Compound V-1 was obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08975434B2uspto-grants-2015_03