HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Tris(1,1-dimethylethyl)phosphine → 9-[3-(4,6-Diphenylpyrimidin-2-yl)phenyl]-9'-phenyl-9H,9'H-[3,3]bicarbazolyl
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Tris(1,1-dimethylethyl)phosphine | HCID 83681 | — |
| Edukt | Sodium t-butoxide | HCID 23676156 | — |
| Edukt | 2-(3-Bromophenyl)-4,6-diphenylpyrimidine | HCID 58943181 | — |
| Edukt | 9-Phenyl-9H,9'H-[3,3']bicarbazolyl | HCID 59306629 | — |
| Katalysator | palladium(II) acetate | HCID 167845 | — |
| Lösungsmittel | P-Xylene | HCID 7809 | — |
| Produkt | 9-[3-(4,6-Diphenylpyrimidin-2-yl)phenyl]-9'-phenyl-9H,9'H-[3,3]bicarbazolyl | HCID 58511489 | — |
Reaktionsschritte
22.00 g (53.86 mmol) of 9-phenyl-9H,9′H-[3,3′]bicarbazolyl 26, 22.93 g (59.24 mmol) of 2-(3-bromophenyl)-4,6-diphenylpyrimidine 14 and 15.81 g (164.47 mmol) of NaOtBu are suspended in 820 ml of p-xylene. 244.79 mg (1.09 mmol) of Pd(OAc)2 and 3.3 ml of a 1M tri-tert-butylphosphine solution are added to this suspension. The reaction mixture is heated under reflux for 19 h. After cooling, the organic phase is separated off, washed three times with 100 ml of water and subsequently evaporated to dryness. The residue is extracted with hot toluene, recrystallised from toluene and finally sublimed in a high vacuum. The yield is 23.10 g (60%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09324954B2 |
| Quelldatensatz | uspto-grants-2016_04 |
| ORD ID | ord-6adf938bce554fbb8bc9c7ee97c9dd54 |
| Quellennotiz | uspto-grants-2016_04 |