Reaction #2122501

Reaction equation

picolinic acid

2-phenylbenzothiazole Iridium chloride

→

impure product

Bis(2-phenylbenzothiazole) Iridium picolinate

Solvents

dichloromethane

Conditions

Workup

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

Procedure

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.

Source