HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
2-Iodoxybenzoic acid → (6-Chloro-imidazo[1,2-b]pyridazin-3-yl)-[2-(2-trimethylsilanyl-ethoxymethyl)-2h-indazol-5-yl]-methanone
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 2-Iodoxybenzoic acid | HCID 108794 | — |
| Edukt | (Rac)-(6-chloro-imidazo[1,2-b]pyridazin-3-yl)-[2-(2-trimethylsilanyl-ethoxymethyl)-2h-indazol-5-yl]-methanol | HCID 87523362 | — |
| Lösungsmittel | Acetone | HCID 180 | — |
| Produkt | (6-Chloro-imidazo[1,2-b]pyridazin-3-yl)-[2-(2-trimethylsilanyl-ethoxymethyl)-2h-indazol-5-yl]-methanone | HCID 87523378 | — |
Reaktionsschritte
(rac)-(6-Chloro-imidazo[1,2-b]pyridazin-3-yl)-[2-(2-trimethylsilanyl-ethoxymethyl)-2H-indazol-5-yl]-methanol (Stage 195.4, 580 mg, 1.349 mmol) was dissolved in acetone (40 mL) and heated 1 h to reflux together with 2-iodoxybenzoic acid (1.133 g, 4.05 mmol). The RM was cooled down to rt and the acetone was removed under reduced pressure. The residue was mixed with 2 M NaOH solution and extracted with EtOAc. The combined organic layers were dried over Na2SO4 and the solvent was evaporated. The residue was purified by flash chromatography (CombiFlash® Companion System®, with RediSep® silica gel column, n-hexane/EtOAc=50:50->0: 100) to afford the title compound as a light brown foam (tR 7.11 min (conditions 3), MH+=428).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08822468B2 |
| Quelldatensatz | uspto-grants-2014_09 |
| ORD ID | ord-31302cce90154816ad01c97c5ad7d61b |
| Quellennotiz | uspto-grants-2014_09 |