Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Cesium carbonate | HCID 10796 | — |
| Edukt | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Edukt | 2-Hydrazinopyridine | HCID 78645 | — |
| Edukt | 2-Fluoro-5-iodobenzaldehyde | HCID 16217058 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 5-iodo-1-pyridin-2-yl-1H-indazole | HCID 59339792 | 5% |
Reaktionsschritte
2-Fluoro-5-iodobenzaldehyde (527 mg, 2.11 mmol), 2-hydrazinopyridine (237 mg, 2.17 mmol), cesium carbonate (2.06 g, 6.32 mmol) and NMP (10 ml) werer charged in a 10 ml vial which was sealed and stirred (magnetic bar) over night at 100° C. Water and ethylacetate were added and the phases was separated. The organic layer was washed three times with brine and concentrated. Purification on silica with ethylacetate:heptane 5:95 to 10:90 over 15 min, 10 ml/min, followed by evaporation afforded 31 mg (5%) of 5-iodo-1-pyridin-2-yl-1H-indazole.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US07728030B2 |
|---|
| Quelldatensatz | uspto-grants-2010_06 |
|---|
| ORD ID | ord-fda5b65fee80468c819f78e9c0b3cf4c |
|---|
| Quellennotiz | uspto-grants-2010_06 |
|---|