Reaktion #2122500

Reaktionsgleichung

8-hydroxyquinoline

2-phenylbenzothiazole Iridium chloride

sodium carbonate

→

Bis(2-phenylbenzothiazole) Iridium (8-hydroxyquinolate)

Ausbeute 57.0%

Lösungsmittel

2-ethoxyethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was heated
2. 2
   Temperaturto reflux under nitrogen in an oil bath overnight (23 hrs.)
3. 3
   SonstigeReaction mixture
4. 4
   Filtrationthe red precipitate was filtered off via vacuum
5. 5
   EinengenThe filtrate was concentrated
6. 6
   workup.ADDITIONmethanol was added
7. 7
   Sonstigeto precipitate more product
8. 8
   FiltrationSuccessive filtrations and precipitations
9. 9
   Sonstigeafforded a 57% yield

Vorschrift

4.7 mmol (0.68 g) of 8-hydroxyquinoline was added to a room-temperature solution of 0.14 mmol 2-phenylbenzothiazole Iridium chloride dimer (0.19 g) in 20 mL of 2-ethoxyethanol. Approximately 700 mg of sodium carbonate was added, and the mixture was heated to reflux under nitrogen in an oil bath overnight (23 hrs.). Reaction mixture was cooled to room temperature, and the red precipitate was filtered off via vacuum. The filtrate was concentrated and methanol was added to precipitate more product. Successive filtrations and precipitations afforded a 57% yield. The emission spectrum is in FIG. 43 and the proton NMR spectrum is in FIG. 44.

Quelle