Reaktion #1740845

ord-2117492620c64e508d70bf691f2e13f7

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe solution was then refluxed for 3 hours
  2. 2
    TemperaturThe reaction mixture was cooled
  3. 3
    Extraktionextracted with methylene chloride
  4. 4
    ExtraktionThe organic extract
  5. 5
    Waschenwas washed with water
  6. 6
    Sonstigewas then collected
  7. 7
    Sonstigedried
  8. 8
    Sonstigeevaporated to dryness
  9. 9
    Sonstigeto obtain a light amber solid (1.8 g; m.p. 113°-118° C.)

Vorschrift

To a freshly prepared solution of sodium ethoxide in ethanol (from 0.35 g sodium metal and 10 ml ethanol) was added 6H-pyrido[3,2,1-de]acridin-1 (2H)-one (1.2 g) portionwise over a period of 10 minutes. To the resulting dark red solution was slowly added diethyl carbonate (1.77 g) and the solution was then refluxed for 3 hours. The reaction mixture was cooled, acidified to pH 2 with concentrated HCl and then extracted with methylene chloride. The organic extract was washed with water and was then collected, dried and evaporated to dryness to obtain a light amber solid (1.8 g; m.p. 113°-118° C.).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05403839uspto-grants-1995_04