反応 #2122500

反応方程式

8-hydroxyquinoline

2-phenylbenzothiazole Iridium chloride

sodium carbonate

→

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

収率 57.0%

溶媒

2-ethoxyethanol

反応条件

後処理

1. 1
   温度the mixture was heated
2. 2
   温度to reflux under nitrogen in an oil bath overnight (23 hrs.)
3. 3
   その他Reaction mixture
4. 4
   ろ過the red precipitate was filtered off via vacuum
5. 5
   濃縮The filtrate was concentrated
6. 6
   workup.ADDITIONmethanol was added
7. 7
   その他to precipitate more product
8. 8
   ろ過Successive filtrations and precipitations
9. 9
   その他afforded a 57% yield

実験手順

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.

出典