Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Dimethylformamide | HCID 6228 | — |
| Edukt | 3-iodo-N,4-dimethylbenzamide | HCID 19688440 | — |
| Katalysator | Zinc cyanide (Zn(CN)2) | HCID 11186 | — |
| Katalysator | HCID 178418397 | HCID 178418397 | — |
| Lösungsmittel | Ammonia ethyl acetate | HCID 18464838 | — |
| Produkt | 3-cyano-N, 4-dimethylbenzamide | HCID 17859780 | — |
Reaktionsschritte
3-Iodo-N, 4-dimethylbenzamide (772 mg), tetrakistriphenylphosphinepalladium (30 mg) and zinc cyanide (250 mg) were suspended in DMF (10 ml) under a nitrogen atmosphere, and the mixture was stirred at 120° C. for 12 hrs. The reaction mixture was diluted with 5% aqueous ammonia-ethyl acetate and the organic layer was washed with water and saturated brine. The organic layer was dried and concentrated, and the residue was subjected to silica gel column chromatography (eluent, hexane:ethyl acetate=2:1–0:1) for purification. The eluate was recrystallized from ethyl acetate-hexane to give the title compound (300 mg) as colorless powder crystals.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07067537B2 |
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| Quelldatensatz | uspto-grants-2006_06 |
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| ORD ID | ord-16e76a07791f45ecb4f4c029730a3c4b |
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| Quellennotiz | uspto-grants-2006_06 |
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