HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethyl 4,6-dichloropyridazine-3-carboxylate → ethyl 4-(6-(1H-pyrazol-1-yl)pyridin-2-ylamino)-6-chloropyridazine-3-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethyl 4,6-dichloropyridazine-3-carboxylate | HCID 53428795 | — |
| Edukt | 2-Amino-6-(1H-pyrazol-1-yl)pyridine | HCID 66520469 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | ethyl 4-(6-(1H-pyrazol-1-yl)pyridin-2-ylamino)-6-chloropyridazine-3-carboxylate | HCID 86689786 | 25% |
Reaktionsschritte
A solution of ethyl 4,6-dichloropyridazine-3-carboxylate (230 mg, 1.04 mmol) and 6-(1H-pyrazol-1-yl)pyridin-2-amine (332.3 mg, 2.07 mmol) in acetonitrile (11.8 mL) was heated at 130° C. in a sealed tube for 48 h, then cooled concentrated in vacuo and then purified by chromatography (silica, Analogix 24 g RediSep Gold column 0 to 20% acetone in dichloromethane, 20 min) to give ethyl 4-(6-(1H-pyrazol-1-yl)pyridin-2-ylamino)-6-chloropyridazine-3-carboxylate (107 mg, 258 μmol, 25%) as a white solid. This material was 83% pure and was used directly in the next step without further purification. MS (EI/CI) m/z: 345.1 [M+H].
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08901124B2 |
| Quelldatensatz | uspto-grants-2014_12 |
| ORD ID | ord-55ea6ac7063b4672acfe0ed385a31610 |
| Quellennotiz | uspto-grants-2014_12 |