反应 #2122500

反应方程式

8-hydroxyquinoline

2-phenylbenzothiazole Iridium chloride

sodium carbonate

→

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

收率 57.0%

溶剂

2-ethoxyethanol

反应条件

后处理

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
   其他Reaction mixture
4. 4
   过滤the red precipitate was filtered off via vacuum
5. 5
   浓缩The filtrate was concentrated
6. 6
   workup.ADDITIONmethanol was added
7. 7
   其他to precipitate more product
8. 8
   过滤Successive filtrations and precipitations
9. 9
   其他afforded a 57% yield

实验过程

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.

来源