تفاعل #2122501

ord-b555fb82be264f68babe54cb639dc92c

معادلة التفاعل

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

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture was heated
  2. 2
    درجة الحرارةto reflux under nitrogen in an oil bath for 8.5 hours
  3. 3
    ترشيحthe yellow precipitate was filtered off via vacuum
  4. 4
    تركيزThe filtrate was concentrated
  5. 5
    workup.ADDITIONmethanol was added
  6. 6
    أخرىto precipitate more product
  7. 7
    ترشيحSuccessive filtrations and precipitations

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08574726B2uspto-grants-2013_11