HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Fluoride → HCID 15856683, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Fluoride | HCID 5235 | — |
| Edukt | Triphenylphosphine | HCID 11776 | — |
| Edukt | Tributylvinyltin | HCID 81998 | — |
| Edukt | 1-Bromo-2,4-difluoro-5-nitrobenzene | HCID 223078 | — |
| Katalysator | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Produkt | HCID 15856683 | HCID 15856683 | 385,6% |
Reaktionsschritte
A mixture of Pd2 dba3 (1.924 g, 2.101 mmol), and PPh3 (2.204 g, 8.404 mmol) was dissolved in toluene (200 mL), degassed and then stirred 10 minutes at ambient temperature. A solution of 1-bromo-2,4-difluoro-5-nitrobenzene (10 g, 42.02 mmol) in toluene (200 mL) was then added to the above solution, followed by tributyl(vinyl)stannane (18.40 mL, 63.03 mmol). The mixture was refluxed for 2 hours, then poured into a mixture of aqueous NaF and diethyl ether. The residue was purified using silica gel column chromatography with 5-10-20% acetone in hexanes to provide 1,5-difluoro-2-nitro-4-vinylbenzene (6 g, 32.41 mmol, 77.13% yield) as yellow oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08754226B2 |
| Quelldatensatz | uspto-grants-2014_06 |
| ORD ID | ord-c0a0e835fffe4cffbb63f0065405a988 |
| Quellennotiz | uspto-grants-2014_06 |