HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Toluene → N'-[3-tert-butyl-1-[[(5R)-5-methyloxolan-2-yl]methyl]pyrazol-5-yl]-N,N-dimethylmethanimidamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Toluene | HCID 1140 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | HCID 178484244 | HCID 178484244 | — |
| Katalysator | Tetraethylammonium Iodide | HCID 6225 | — |
| Katalysator | Tetrabutylammonium Iodide | HCID 67553 | — |
| Katalysator | Tetrabutylammonium hydrogen sulfate | HCID 94433 | — |
| Produkt | N'-[3-tert-butyl-1-[[(5R)-5-methyloxolan-2-yl]methyl]pyrazol-5-yl]-N,N-dimethylmethanimidamide | HCID 87439811 | 25% |
Reaktionsschritte
To a solution of Example 63A (1.6 g, 8.2 mmol) in toluene (100 mL) were added potassium carbonate (2.3 g, 16.5 mmol), Example 64B (2.7 g, 9.9 mmol), tetrabutylammonium iodide (70 mg), tetraethylammonium iodide (70 mg) and tetrabutylammonium hydrogensulfate (70 mg). The reaction mixture was refluxed for 16 h, cooled, filtered and concentrated under reduced pressure. The residue was purified by column chromatography using an Analogix® Intelliflash280™ (SiO2, 0-10% methanol in dichloromethane) to provide 0.6 g (25%) of the title compound. MS (ESI+) m/z 293 (M+H)+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08492371B2 |
| Quelldatensatz | uspto-grants-2013_07 |
| ORD ID | ord-a1fb895377e843209297d16749b98ef0 |
| Quellennotiz | uspto-grants-2013_07 |