HuagongsheHuagongshe Chemistry Print Report · For research reference only
Carbazole → 1-Phenyl-9H-carbazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Carbazole | HCID 6854 | — |
| Reactant | Iodobenzene | HCID 11575 | — |
| Reactant | sodium 2-methylpropan-2-olate | HCID 178418730 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | 1-Phenyl-9H-carbazole | HCID 13497474 | 84.1% |
Reaction Steps
In a stream of argon, 670 g of carbazole, 850 kg of iodobenzene, 20 L of xylene, 460 g of t-BuONa, and palladium acetate (Pd(OAc)2) were loaded, and then the mixture was refluxed for 8 hours. Impurities were filtrated, and then the filtrate was concentrated under reduced pressure and washed with hexane. After that, the washed product was dried. As a result, 820 g of phenylcarbazole were obtained as a white powder. A reaction was performed in the same manner as in the synthesis of Intermediate 1-1 except that phenylcarbazole was used instead of 4-bromobiphenyl. As a result, 650 g of a white powder were obtained. The powder was identified as Intermediate 1-11 by FD-MS analysis.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09054322B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-aa49f7d7daea4032ab4f92bc14f66ac7 |
| Source note | uspto-grants-2015_06 |