반응 #2122500

반응 방정식

8-hydroxyquinoline

2-phenylbenzothiazole Iridium chloride

sodium carbonate

→

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

수율 57.0%

용매

2-ethoxyethanol

반응 조건

후처리

1. 1
   온도the mixture was heated
2. 2
   온도to reflux under nitrogen in an oil bath overnight (23 hrs.)
3. 3
   기타Reaction mixture
4. 4
   여과the red precipitate was filtered off via vacuum
5. 5
   농축The filtrate was concentrated
6. 6
   workup.ADDITIONmethanol was added
7. 7
   기타to precipitate more product
8. 8
   여과Successive filtrations and precipitations
9. 9
   기타afforded a 57% yield

실험 절차

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.

출처