Reaktion #937948

ord-29ce2678844b4085ae179ee64ebefe80

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGThe mixture was stirred at room temperature for 12 hours
  2. 2
    Sonstigethe crystals precipitated
  3. 3
    Filtrationwere recovered by filtration
  4. 4
    SonstigeThe crude crystals were purified by silica gel flash column chromatography (eluent: methylene chloride containing 1% methanol)

Vorschrift

10-bromo-2-hydroxy-4H-pyrido[3,2,1-jk]carbazole-4-one (3 g) obtained in Example 59 was suspended in dimethyl sulfoxide (120 ml), and potassium carbonate (2.6 g) was added to the suspension. The mixture was stirred at room temperature for 30 minutes and i-propyl bromoacetate (1.4 ml) and potassium iodide (1 grain) were added in succession to the mixture. The mixture was stirred at room temperature for 12 hours, and the reaction mixture was poured into ice water (500 ml), and the crystals precipitated were recovered by filtration. The crude crystals were purified by silica gel flash column chromatography (eluent: methylene chloride containing 1% methanol) to obtain the title compound (2.0 g, 51%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06018046uspto-grants-2000_01