HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethylformamide → HCID 117690933, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethylformamide | HCID 6228 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 1-Ethynyl-4-(trifluoromethoxy)benzene | HCID 2778494 | — |
| Edukt | 3-Iodo[1,4]benzodioxino[2,3-c]pyridazine | HCID 89584640 | — |
| Katalysator | Copper iodide | HCID 83717 | — |
| Katalysator | HCID 178419050 | HCID 178419050 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | HCID 117690933 | HCID 117690933 | — |
Reaktionsschritte
To a sealed reaction container were added 3-iodo[1,4]benzodioxino[2,3-c]pyridazine (200 mg) synthesized in Production Example 9 to be mentioned later, 4-ethynylphenyl trifluoromethyl ether (0.15 mL), copper iodide (6 mg), triethylamine (64 mg), bis(triphenylphosphine)palladium (II) dichloride (22 mg) and dimethylformamide (5 mL), and the mixture was stirred at 120° C. for 0.5 hr. Ethyl acetate and water were added, the organic layer was dried over anhydrous sodium sulfate, and the solvent was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane-ethyl acetate) to give 3-{[4-(trifluoromethoxy)phenyl]ethynyl}[1,4]benzodioxino[2,3-c]pyridazine (100 mg).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09212147B2 |
| Quelldatensatz | uspto-grants-2015_12 |
| ORD ID | ord-5d3a84ecd16b40b1a5150ca533ed6a41 |
| Quellennotiz | uspto-grants-2015_12 |