Реакция #2122501

ord-b555fb82be264f68babe54cb639dc92c

Уравнение реакции

O=C(O)c1ccccn1
picolinic acid
[Cl][Ir]([Cl])[Cl].c1ccc(-c2nc3ccccc3s2)cc1
2-phenylbenzothiazole Iridium chloride
O=C([O-])c1ccccn1.O=C([O-])c1ccccn1.O=C([O-])c1ccccn1.[Ir+3].c1ccc(-c2nc3ccccc3s2)cc1.c1ccc(-c2nc3ccccc3s2)cc1
impure product
O=C([O-])c1ccccn1.O=C([O-])c1ccccn1.O=C([O-])c1ccccn1.[Ir+3].c1ccc(-c2nc3ccccc3s2)cc1.c1ccc(-c2nc3ccccc3s2)cc1
Bis(2-phenylbenzothiazole) Iridium picolinate

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe mixture was heated
  2. 2
    Температураto reflux under nitrogen in an oil bath for 8.5 hours
  3. 3
    Фильтрацияthe yellow precipitate was filtered off via vacuum
  4. 4
    КонцентрированиеThe filtrate was concentrated
  5. 5
    workup.ADDITIONmethanol was added
  6. 6
    Другоеto precipitate more product
  7. 7
    ФильтрацияSuccessive filtrations and precipitations

Методика

2.14 mmol (0.26 g) of picolinic acid was added to a room-temperature solution of 0.80 mmol 2-phenylbenzothiazole Iridium chloride dimer (1.0 g) in 60 mL of dichloromethane. The mixture was heated to reflux under nitrogen in an oil bath for 8.5 hours. The reaction mixture was cooled to room temperature, and the yellow precipitate was filtered off via vacuum. The filtrate was concentrated and methanol was added to precipitate more product. Successive filtrations and precipitations yielded about 900 mg of impure product. Emission spectrum is in FIG. 45.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08574726B2uspto-grants-2013_11