Reaktion #90067

ord-6ea983a8eeac40a4bd002d1102536314

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionwas then extracted with ethyl acetate
  2. 2
    WaschenThe organic layer was washed with brine
  3. 3
    Trocknendried over magnesium sulfate
  4. 4
    SonstigeThe solids obtained
  5. 5
    Filtrationafter filtration and concentration under reduced pressure
  6. 6
    Waschenwere washed with dichloromethane
  7. 7
    Sonstigepurified by HPLC

Vorschrift

(3-Cyano-8-methoxy-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazol-9-yl)-propynoic acid methyl ester (Compound E6-1, 15.2 mg, 0.038 mmol) was dissolved in a mixture solvent of methanol (1.5 mL) and THF (0.5 mL), added with 2 N aqueous solution of potassium hydroxide (5 drops), and then stirred at room temperature overnight. 0.5 N Hydrochloric acid was added to the reaction solution, which was then extracted with ethyl acetate. The organic layer was washed with brine and dried over magnesium sulfate. The solids obtained after filtration and concentration under reduced pressure were washed with dichloromethane and purified by HPLC to obtain the title compound (white solid, 9.6 mg, 66%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09440922B2uspto-grants-2016_09