Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Sodium Sulfide | HCID 14804 | — |
| Edukt | 4-(3-Fluoropyridin-4-yl)benzonitrile | HCID 10856435 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 4-(3-Mercaptopyridin-4-yl)benzonitrile | HCID 67997061 | 96% |
Reaktionsschritte
A mixture of 4-(3-fluoropyridin-4-yl)benzonitrile (1.08 g, 5.4 mmol) and sodium sulfide (0.84 g, 10.8 mmol) in DMF (20 mL) was stirred at 130° C. for 0.5 hours. While the reaction was cooled in ice water bath, aqueous HCl (6N, 2.5 mL) was added drop wise with rigorous stirring. The resulting yellow paste was concentrated using rotary evaporation on a water bath (80° C.) to dryness. The resulting yellow solid was extracted with methanol (4×20 mL). The combined extracts were concentrated to dryness to give a yellow solid (1.1 g, 96%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08629278B2 |
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| Quelldatensatz | uspto-grants-2014_01 |
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| ORD ID | ord-cc55aeea824d4cfabb0fc277184748da |
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| Quellennotiz | uspto-grants-2014_01 |
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