Reaktion #2122501

ord-b555fb82be264f68babe54cb639dc92c

Reaktionsgleichung

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

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture was heated
  2. 2
    Temperaturto reflux under nitrogen in an oil bath for 8.5 hours
  3. 3
    Filtrationthe yellow precipitate was filtered off via vacuum
  4. 4
    EinengenThe filtrate was concentrated
  5. 5
    workup.ADDITIONmethanol was added
  6. 6
    Sonstigeto precipitate more product
  7. 7
    FiltrationSuccessive filtrations and precipitations

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08574726B2uspto-grants-2013_11