HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Iodine → HCID 178477832, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Iodine | HCID 807 | — |
| Edukt | Potassium Hydroxide | HCID 14797 | — |
| Edukt | 5,6-dichloro-1H-indazole | HCID 412303 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | HCID 178477832 | HCID 178477832 | 99% |
Reaktionsschritte
To a solution of 5,6-dichloro-1H-indazole (0.50 g, 2.67 mmol) in DMF (8 ml) at room temperature was added powdered potassium hydroxide (450 mg, 8.02 mmol) and iodine (1.02 g, 4.01 mmol). The maroon reaction mixture was stirred at room temperature for 45 min then quenched with 10% aqueous Na2S2O3 and diluted with water. The mixture was extracted with EtOAc (2×). The combined organics were washed with water (3×), dried over MgSO4 and concentrated to afford 827 mg (99%) of 5,6-dichloro-3-iodo-1H-indazole as a pale yellow solid. 1H NMR (DMSO-d6, 400 MHz): δ (ppm) 13.79 (s, 1H), 7.94 (s, 1H), 7.72 (s, 1H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08658646B2 |
| Quelldatensatz | uspto-grants-2014_02 |
| ORD ID | ord-091bfeade6204eedbc853379d096cb9f |
| Quellennotiz | uspto-grants-2014_02 |