HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Iodine → HCID 178451733, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Iodine | HCID 807 | — |
| Edukt | Potassium Hydroxide | HCID 14797 | — |
| Edukt | Sodium Thiosulfate | HCID 24477 | — |
| Edukt | 4-(1H-indazol-6-yl)-3,6-dihydro-2H-pyridine-1-carboxylic acid tert-butyl ester | HCID 67449416 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | HCID 178451733 | HCID 178451733 | — |
Reaktionsschritte
A solution of 4-(1H-indazol-6-yl)-3,6-dihydro-2H-pyridine-1-carboxylic acid tert-butyl ester (9.70 g, 3.24 mmol) in DMF (32 mL) at room temperature was treated with iodine (1.23 g, 4.86 mmol) and KOH (grounded, 454 mg, 8.1 mmol). The resulting mixture was stirred at room temperature for 40 min, then treated with saturated Na2S2O3 aqueous solution. The resulting mixture was then extracted with EtOAc (3×). The combined extracts were washed with brine and dried over Na2SO4. The resulting mixture was filtered and concentration under reduced pressure. The resulting residue was purified by flash chromatography on silica-gel (gradient eluant 10% to 40% EtOAc in heptane) to yield the title compound as white solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08822447B2 |
| Quelldatensatz | uspto-grants-2014_09 |
| ORD ID | ord-98c16b4a4f534f93ada601a2380dd571 |
| Quellennotiz | uspto-grants-2014_09 |