Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | 2-Bromoselenophene | HCID 137013 | — |
| Edukt | HCID 59456333 | HCID 59456333 | — |
| Katalysator | HCID 178418397 | HCID 178418397 | — |
| Lösungsmittel | Toluene ethanol | HCID 21863594 | — |
| Produkt | HCID 59456349 | HCID 59456349 | — |
Reaktionsschritte
A mixture of 8.9 g (42.4 mmol) of 2-bromoselenophene, 16.0 g (59.7 mmol) of 4-(4-ethylcyclohexyl)-2,3-difluorophenylboronic acid, 3.93 g (3.40 mmol) of tetrakis(triphenylphosphine)palladium(0) and 125 ml of 2 N sodium carbonate soln. in 600 ml of toluene/ethanol (1:1) is heated under reflux for 20 h. After cooling, the organic phase is separated off, and the aqueous phase is extracted with toluene. The combined organic phases are washed with sat. sodium chloride soln., and the solution is dried using sodium sulfate. The solution is concentrated to dryness, and the residue is purified by column chromatography (SiO2, toluene). The further purification is carried out by recrystallisation from n-heptane:EtOH=1:1 and IPA. 2-[4-(4-Ethylcyclohexyl)-2,3-difluorophenyl]selenophene is obtained as a pale-yellowish solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08304036B2 |
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| Quelldatensatz | uspto-grants-2012_11 |
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| ORD ID | ord-9141115f49904b5e9db82f30946f0890 |
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| Quellennotiz | uspto-grants-2012_11 |
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