Reaktion #68684

Reaktionsgleichung

2-bromo-13,13-dimethyl-6,11-di(naphthalen-2-yl)-11,13-dihydro-6H-indeno[1,2-b]anthracene-6,11-diol

Sodium hypophosphite

→

2-bromo-13,13-dimethyl-6,11-di(naphthalen-2-yl)-13H-indeno[1,2-b]anthracene

Ausbeute 76.0%

Lösungsmittel

acetic acid

Reaktionsbedingungen

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

2-bromo-13,13-dimethyl-6,11-di(naphthalen-2-yl)-11,13-dihydro-6H-indeno[1,2-b]anthracene-6,11-diol (5 g, 0.0075 mol), KI (12.45 g, 0.075 mol), and Sodium hypophosphite (6 g, 0.037 mol) were placed in a flask, and acetic acid (200 ml) was added thereto. 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 2-bromo-13,13-dimethyl-6,11-di(naphthalen-2-yl)-13H-indeno[1,2-b]anthracene (3.56 g, yield=76%).

Quelle