HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tris(1,1-dimethylethyl)phosphine → Carbazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tris(1,1-dimethylethyl)phosphine | HCID 83681 | — |
| Reactant | Sodium t-butoxide | HCID 23676156 | — |
| Reactant | HCID 67466017 | HCID 67466017 | — |
| Catalyst | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | Carbazole | HCID 6854 | — |
Reaction Steps
6.5 g (23 mmol) of 5-amino-7b-azabenzo[e]acephenanthrylen-8-one, 7.1 g (23 mmol) of 2,2′-dibromodiphenyl, 16 g (72 mmol) of NaOtBu, 1.4 g (1.58 mmol) of Pd2 dba3 and 6.3 ml (6.3 mmol) of t-Bu3P are heated at 110° C. for 36 h in 150 ml of toluene under a protective-gas atmosphere. After cooling, the precipitated solid is filtered off with suction, washed with water and ethanol and dried. The residue is extracted with hot toluene, recrystallised from toluene and finally sublimed in a high vacuum. The yield after sublimation is 7 g (16 mmol, 71%) with a purity of 99.9%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09139582B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-3ec813d4ec134e1bb46e6030e3644574 |
| Source note | uspto-grants-2015_09 |