تفاعل #2122500
ord-1cc428ed83a1499ea7e895a2b44d59df
معادلة التفاعل
8-hydroxyquinoline
2-phenylbenzothiazole Iridium chloride
sodium carbonate
→
Bis(2-phenylbenzothiazole) Iridium (8-hydroxyquinolate)
المردود 57.0%
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةthe mixture was heated
- 2درجة الحرارةto reflux under nitrogen in an oil bath overnight (23 hrs.)
- 3أخرىReaction mixture
- 4ترشيحthe red precipitate was filtered off via vacuum
- 5تركيزThe filtrate was concentrated
- 6workup.ADDITIONmethanol was added
- 7أخرىto precipitate more product
- 8ترشيحSuccessive filtrations and precipitations
- 9أخرىafforded a 57% yield
الإجراء التجريبي
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.