反应 #2122501

ord-b555fb82be264f68babe54cb639dc92c

反应方程式

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

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The mixture was heated
  2. 2
    温度to reflux under nitrogen in an oil bath for 8.5 hours
  3. 3
    过滤the yellow precipitate was filtered off via vacuum
  4. 4
    浓缩The filtrate was concentrated
  5. 5
    workup.ADDITIONmethanol was added
  6. 6
    其他to precipitate more product
  7. 7
    过滤Successive filtrations and precipitations

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08574726B2uspto-grants-2013_11