Reaktion #68691

Reaktionsgleichung

13,13-dimethyl-6H-indeno[1,2-b]anthracene-6,11(13H)-dione

HI

iodine

→

13,13-dimethyl-13H-indeno[1,2-b]anthracene

Ausbeute 58.6%

Lösungsmittel

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturunder reflux for 48 hours
2. 2
   SonstigeAfter the reaction was terminated
3. 3
   workup.ADDITIONthe reaction solution was added with distilled water (500 ml)
4. 4
   FiltrationThen, the resultant solid was filtered
5. 5
   workup.DISSOLUTIONdissolved in toluene (200 ml)
6. 6
   workup.STIRRINGThe reaction mixture was stirred
7. 7
   Temperaturunder reflux for 3 hours
8. 8
   SonstigeAfter the reaction was terminated
9. 9
   Extraktionthe reaction solution was extracted
10. 10
    Sonstigepurified by column chromatography

Vorschrift

13,13-dimethyl-6H-indeno[1,2-b]anthracene-6,11(13H)-dione (19 g, 0.058 mol) was dissolved in acetic acid (200 ml) and 57% HI (50 ml) was added thereto. The reaction mixture was stirred under reflux for 48 hours. After the reaction was terminated, the reaction solution was added with distilled water (500 ml). Then, the resultant solid was filtered and dissolved in toluene (200 ml), and iodine (4.56 g, 0.018 mol) was added thereto. The reaction mixture was stirred under reflux for 3 hours. After the reaction was terminated, the reaction solution was extracted and purified by column chromatography to give 13,13-dimethyl-13H-indeno[1,2-b]anthracene (10 g, yield=58%).

Quelle