Reaktion #67966

ord-a0777cb54b1d450bad63f798dfc6ee12

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was removed under reduced pressure, water and chloroform
  2. 2
    workup.ADDITIONwas added
  3. 3
    workup.STIRRINGstirred for 2 hours
  4. 4
    SonstigeThe organic layer was separated
  5. 5
    Extraktionthe aqueous layer was extracted with chloroform
  6. 6
    Waschenthe resultant solution was washed sequentially with water
  7. 7
    Trocknenan aqueous saturated sodium chloride solution and dried over anhydrous magnesium sulfate
  8. 8
    Sonstigethe solvent was removed under reduced pressure

Vorschrift

To 0.56 g of 1-(1,3-dioxolan-2-ylmethyl)-7-methoxyquinolin-2(1H)-one, 5.6 mL of a 90% aqueous trifluoroacetic acid solution was added, the mixture was stirred at room temperature for 2 hours. The solvent was removed under reduced pressure, water and chloroform was added thereto, and the reaction mixture was adjusted to pH 7.0 with an aqueous saturated sodium hydrogen carbonate solution and stirred for 2 hours. The organic layer was separated, and the aqueous layer was extracted with chloroform. The organic layer and the extract were combined, the resultant solution was washed sequentially with water and an aqueous saturated sodium chloride solution and dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure to obtain 0.36 g of a yellow oily substance, (7-methoxy-2-oxoquinolin-1(2H)-yl)acetaldehyde.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524738B2uspto-grants-2013_09