HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Cesium carbonate → 5-(4-iodo-2-methyl-imidazol-1-yl)-2-methyl-2H-pyridazin-3-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Cesium carbonate | HCID 10796 | — |
| Edukt | 5-Chloro-2-methylpyridazin-3(2H)-one | HCID 12910144 | — |
| Edukt | HCID 178433060 | HCID 178433060 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 5-(4-iodo-2-methyl-imidazol-1-yl)-2-methyl-2H-pyridazin-3-one | HCID 66865685 | 71,3% |
Reaktionsbedingungen
| Temperatur | 45 °C |
|---|
Reaktionsschritte
To a solution of 160 mg (1.11 mmol) of 5-chloro-2-methyl-2H-pyridazin-3-one (CAS: [14628-34-3]), 230 mg (1.11 mmol) of 4-iodo-2-methyl-1H-imidazole (CAS: [73746-45-9]), in 3.5 ml of dry DMF were added 721 mg (2.21 mmol) of cesium carbonate. The suspension was stirred for 30 min at 45° C., then for 3 h at 65° C. and allowed to cool. The cristallised product is filtered off, washed with ethyl acetate and dried in vaccuo to yield 250 mg (0.791 mmol, 71%) of the title compound as a crystalline light yellow solid, MS: m/e=316.9 (M+H+).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08334287B2 |
| Quelldatensatz | uspto-grants-2012_12 |
| ORD ID | ord-fb33a895c6bf45c08330c5a5f7d30a76 |
| Quellennotiz | uspto-grants-2012_12 |