Reaktion #68687

ord-325e201e805644599f1aa2cb08829680

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwhile heating
  2. 2
    SonstigeAfter the reaction was terminated
  3. 3
    workup.ADDITIONthe reaction solution was added to an excess of distilled water
  4. 4
    WaschenThe resultant solid was washed with distilled water
  5. 5
    Filtrationfiltered
  6. 6
    Sonstigepurified by column chromatography

Vorschrift

9-bromo-13,13-dimethyl-6,11-diphenyl-11,13-dihydro-6H-indeno[1,2-b]anthracene-6,11-diol (4.19 g, 0.0075 mol), potassium iodide (12.45 g, 0.075 mol), and sodium hypophosphite (6 g, 0.037 mol) were placed in a flask, and were suspended in acetic acid (200 ml). The reaction mixture was stirred for five hours while heating. After the reaction was terminated, the reaction solution was added to an excess of distilled water. The resultant solid was washed with distilled water, filtered, and purified by column chromatography to give 9-bromo-13,13-dimethyl-6,11-diphenyl-13H-indeno[1,2-b]anthracene (2.9 g, yield=74%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08525158B2uspto-grants-2013_09