Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Sodium Sulfide | HCID 14804 | — |
| Edukt | N-{4-[2-Amino-3,5-dicyano-6-(phenylsulphanyl)-4-pyridinyl]phenyl}acetamide | HCID 12016387 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | HCID 178474088 | HCID 178474088 | — |
Reaktionsschritte
30.83 g (80 mmol) of N-{4-[2-amino-3,5-dicyano-6-(phenylsulphanyl)-4-pyridinyl]-phenyl}-acetamide are dissolved in 120 ml of DMF under argon, after which 9.36 g (120 mmol) of sodium sulphide are added and the mixture is stirred at 80° C. for 2 hours. A solution of 20 ml of 1N aqueous HCl in 44 ml of water is then added dropwise at from 40 to 65° C., after which the crystals which have formed during this procedure are filtered off with suction and washed with water. The precipitate is suspended in 200 ml of methanol and stirred under reflux for 5 minutes. After cooling down to room temperature, the precipitate is filtered off with suction, washed with methanol and diethyl ether and dried in vacuo.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07045631B2 |
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| Quelldatensatz | uspto-grants-2006_05 |
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| ORD ID | ord-4f161f2e2bce41638cfba2803df8ea0a |
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| Quellennotiz | uspto-grants-2006_05 |
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