HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Carbonate → Diisopropyl(((2-((2-methoxyphenyl)carbamoyl)-3-((4-nitro-phenyl)thio)phenyl)amino)methyl)phosphonate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | Diisopropyl bromomethylphosphonate | HCID 4366885 | — |
| Edukt | 2-amino-N-(2-methoxyphenyl)-6-(4-nitrophenyl-thio)benzamide | HCID 71811587 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | Diisopropyl(((2-((2-methoxyphenyl)carbamoyl)-3-((4-nitro-phenyl)thio)phenyl)amino)methyl)phosphonate | HCID 71811718 | 41% |
Reaktionsbedingungen
| Temperatur | 60 °C |
|---|
Reaktionsschritte
Compound 25 (1.0 equiv.) was dissolved in MeCN (40 mL) and treated with anhydrous potassium carbonate (2.0 equiv.) at room temperature. To this mixture diisopropyl(bromomethyl)phosphonate (1.2 equiv.) was added via a micro syringe. After being stirred for 4 Hours at 60° C., the reaction mixture was concentrated under reduced pressure. The crude residue was diluted by ethyl acetate (50 mL), and washed with water (2×10 mL). Then it was dried over anhydrous Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (1:4 v/v ethyl acetate/petroleum ether) to provide a yellow solid (235.2 mg, 41% yield).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09402819B2 |
| Quelldatensatz | uspto-grants-2016_08 |
| ORD ID | ord-88db3d8f35ff41cca758454c7100483a |
| Quellennotiz | uspto-grants-2016_08 |