Reaktion #67996

ord-299eb1dba0ef4f03a1bcc0dc4180e47e

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was removed under reduced pressure
  2. 2
    Extraktionextracted with ethyl acetate
  3. 3
    WaschenThe organic layer was washed 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

Into 5 mL of a 90% aqueous trifluoroacetic acid solution, 350 mg of methyl 1-(1,3-dioxolan-2-ylmethyl)-7-methoxy-2-oxo-1,2-dihydroquinoline-5-carboxylate was dissolved, and the mixture was stirred at room temperature overnight. The solvent was removed under reduced pressure, and the resultant solution was alkalified with an aqueous saturated sodium hydrogen carbonate solution, and then extracted with ethyl acetate. The organic layer 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 476 mg of a pale yellow oily substance, methyl 7-methoxy-2-oxo-1-(2-oxoethyl)-1,2-dihydroquinoline-5-carboxylate.

Quelle

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