Reaktion #67976

ord-f6506e59d57740879b99cbf6379f5255

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.WAITstood still at room temperature for 14 hours
  2. 2
    SonstigeThe organic layer was separated
  3. 3
    Waschenwashed sequentially with water
  4. 4
    Trocknenan aqueous saturated sodium chloride solution and dried over anhydrous magnesium sulfate
  5. 5
    Sonstigethe solvent was removed under reduced pressure

Vorschrift

To 95 mg of 7-(cyclopropoxy)-1-(1,3-dioxolan-2-ylmethyl)-4-methylquinolin-2(1H)-one, 1.5 mL of an 80% aqueous trifluoroacetic acid solution was added, the mixture was stirred at room temperature for 6 hours, and then stood still at room temperature for 14 hours. Thereto were added ethyl acetate and water, and the mixture was neutralized with an aqueous saturated sodium hydrogen carbonate solution and an aqueous sodium hydroxide solution. The organic layer was separated, 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 84 mg of a yellow oily substance, (7-(cyclopropoxy)-4-methyl-2-oxo-1,2-dihydroquinolin-1-yl)acetaldehyde.

Quelle

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