HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Nitrogen → 6-Anthracen-9-ylphenanthrene-9-carboxylic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Nitrogen | HCID 947 | — |
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | 6-Bromophenanthrene-9-carboxylic acid | HCID 289464 | — |
| Edukt | 9-Anthraceneboronic Acid | HCID 15510213 | — |
| Katalysator | HCID 178418397 | HCID 178418397 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Lösungsmittel | Methanol--water (1/1) | HCID 22242641 | — |
| Produkt | 6-Anthracen-9-ylphenanthrene-9-carboxylic acid | HCID 59629491 | — |
Reaktionsschritte
32.86 g (148 mmol) of anthracene-9-boronic acid, 37.2 g (124 mmol) of 6-bromophenanthrene-9-carboxylic acid and 220 ml of 2 M Na2CO3 solution are suspended in 1 l of toluene and 1 l of EtOH, the mixture is saturated with N2, 2.9 g (3 mmol) of tetrakis(triphenylphosphine)palladium(0) are added, and the mixture is heated at the boil for 2 h. The mixture is poured into 3 l of a mixture of water/MeOH/6 M HCl 1:1:1, and the beige precipitate is filtered off with suction, washed with water, EtOH and toluene and dried. The content of product according to 1H-NMR is about 96% with an overall yield of 38.5 g (78%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08993123B2 |
| Quelldatensatz | uspto-grants-2015_03 |
| ORD ID | ord-3ebbd0e323584a6d9b3fabd3922fed03 |
| Quellennotiz | uspto-grants-2015_03 |