Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Formamide | HCID 713 | — |
| Edukt | Imidazole | HCID 795 | — |
| Edukt | Diethylene glycol dibutyl ether | HCID 8210 | — |
| Edukt | Benzene, 1-bromo-3-(trifluoromethyl)- | HCID 9817 | — |
| Edukt | Triphenylphosphine | HCID 11776 | — |
| Katalysator | Dichlorobis(triphenylphosphine)palladium | HCID 6102075 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Produkt | m-(Trifluoromethyl)benzamide | HCID 74535 | — |
Reaktionsschritte
0.491 g of bis(triphenylphosphine)-palladium(II)chloride, 0.371 g of triphenylphosphine and 2.6 g of imidazole are placed in a 200 ml glass autoclave, and then 8.01 g of 3-(trifluoromethyl)bromobenzene, 25 ml of formamide and 810.3 mg of diethylene glycol dibutylether are added as an internal gas chromatography (GC) standard. The autoclave is closed, flushed with nitrogen three times and then 5 bars carbon monoxide are applied. The reaction mixture is heated to 120° C. and stirred for 14 hours. The mixture is then cooled and the content determined by GC (0.8 ml of reaction mixture mixed with 5 ml of water, then 2 ml of diethylether added, and GC determination effected with the organic phase). The yield of title compound is 82% by weight.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US06441233B1 |
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| Quelldatensatz | uspto-grants-2002_08 |
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| ORD ID | ord-6b3dc407506d4a38a3ba8739779bc9a8 |
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| Quellennotiz | uspto-grants-2002_08 |
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