HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 4-(4-Amino-phenylsulfanyl)-N-(4-bromo-phenyl)-3-nitro-benzamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Cesium carbonate | HCID 10796 | — |
| Edukt | 4-Aminothiophenol | HCID 14510 | — |
| Edukt | N-(4-bromophenyl)-4-chloro-3-nitrobenzamide | HCID 1068537 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 4-(4-Amino-phenylsulfanyl)-N-(4-bromo-phenyl)-3-nitro-benzamide | HCID 67040850 | 96% |
Reaktionsschritte
A solution of the product from Example 10A (3.0 g, 8.44 mmol), 4-aminothiophenol (1.06 g, 8.44 mmol) and cesium carbonate (5.5 g, 17.0 mmol) in N,N-dimethylformamide (15 mL) was heated to 90° C. for 4 hours. After cooling to room temperature the mixture was poured into ice water (100 mL) and the resultant solution acidified to pH 5 with 1N aqueous hydrochloric acid. The solution was then extracted with ethyl acetate (3×50 mL), the combined extracts dried over sodium sulfate, filtered and concentrated under vacuum to provide the title compound as an orange solid (3.6 g, 96%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07910595B2 |
| Quelldatensatz | uspto-grants-2011_03 |
| ORD ID | ord-267650fa143b451f829bc3cb6156fe0a |
| Quellennotiz | uspto-grants-2011_03 |