Reaktion #68688

ord-f685fddc85a44e5698379e61393ca7bf

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
  5. 5
    Filtrationfiltered
  6. 6
    Sonstigepurified by column chromatography

Vorschrift

9-bromo-13,13-dimethyl-6,11-di(naphthalen-2-yl)-11,13-dihydro-6H-indeno[1,2-b]anthracene-6,11-diol (11.87 g, 0.018 mol), Potassium iodide (29.88 g, 0.18 mol), and Sodium hypophosphite (35.63 g, 0.297 mol) were placed in a flask, and were suspended in acetic acid (300 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, filtered and purified by column chromatography to give 9-bromo-13,13-dimethyl-6,11-di(naphthalen-2-yl)-13H-indeno[1,2-b]anthracene (8 g, yield=71%).

Quelle

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