Реакция #2122500

Уравнение реакции

8-hydroxyquinoline

2-phenylbenzothiazole Iridium chloride

sodium carbonate

→

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

Выход 57.0%

Растворители

2-ethoxyethanol

Условия реакции

Обработка

1. 1
   Температураthe mixture was heated
2. 2
   Температураto reflux under nitrogen in an oil bath overnight (23 hrs.)
3. 3
   ДругоеReaction mixture
4. 4
   Фильтрацияthe red precipitate was filtered off via vacuum
5. 5
   КонцентрированиеThe filtrate was concentrated
6. 6
   workup.ADDITIONmethanol was added
7. 7
   Другоеto precipitate more product
8. 8
   ФильтрацияSuccessive filtrations and precipitations
9. 9
   Другоеafforded a 57% yield

Методика

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.

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