Reacción #2122501

ord-b555fb82be264f68babe54cb639dc92c

Ecuación de reacción

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

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaThe mixture was heated
  2. 2
    Temperaturato reflux under nitrogen in an oil bath for 8.5 hours
  3. 3
    Filtraciónthe yellow precipitate was filtered off via vacuum
  4. 4
    ConcentraciónThe filtrate was concentrated
  5. 5
    workup.ADDITIONmethanol was added
  6. 6
    Otroto precipitate more product
  7. 7
    FiltraciónSuccessive filtrations and precipitations

Procedimiento

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.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08574726B2uspto-grants-2013_11