Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Potassium Hydroxide | HCID 14797 | — |
| Edukt | 2-Chloro-3-nitropyridine | HCID 79613 | — |
| Edukt | Thiourea | HCID 2723790 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | HCID 178526679 | HCID 178526679 | — |
Reaktionsschritte
2-mercapto-3-nitropyridine was prepared by treating 3-nitro-2-chloro-pyridine (50 g, 0.0317 mol) with thiourea (24 g, 0.0317 mol) in 200 mL of ethanol at reflux for several hours. After the reaction mixture was allowed to cool, 7.19 mL solution of KOH (42.8 g in 115 mL of water) was added and the resulting mixture was heated at reflux for 3 hours. The crude reaction mixture was cooled to room temperature and then concentrated to 50% of its volume in vacuo. After diluting with 300 mL of water, the product was isolated by vacuum filtration as an orange solid that was used without further purification. MS (DCI/NH3) m/z 157 (M+H)+. 1H NMR (300 MHz, DMSO-d6) δ 5.76 (m, 1H), 7.67 (dd, J=8.46, 4.78 Hz, 1H), 8.63 (dd, J=8.46, 1.47 Hz, 1H), 8.73 (dd, J=4.60, 1.65 Hz, 1H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07902203B2 |
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| Quelldatensatz | uspto-grants-2011_03 |
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| ORD ID | ord-75cc0655452c4bdea50cfd6e5a58c3ef |
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| Quellennotiz | uspto-grants-2011_03 |
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