HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
4-Aminothiophenol → 4-(4-Amino-phenylsulfanyl)-N-(4-bromo-phenyl)-3-nitro-benzamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 4-Aminothiophenol | HCID 14510 | — |
| Edukt | Sodium Acetate | HCID 517045 | — |
| Edukt | N-(4-bromophenyl)-4-chloro-3-nitrobenzamide | HCID 1068537 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | 4-(4-Amino-phenylsulfanyl)-N-(4-bromo-phenyl)-3-nitro-benzamide | HCID 67040850 | 87,2% |
Reaktionsschritte
A mixture of the product of Example 10A (1.00 g, 2.816 mmol), 4-aminothiophenol (529 mg, 4.224 mmol) and anhydrous sodium acetate (1.155 g, 14.08 mmol) in anhydrous ethanol (30 mL) was heated at reflux under a nitrogen atmosphere for 19 hours. The reaction was cooled to room temperature and the ethanol removed by rotary evaporation. The residue was taken up in water (50 mL) and extracted with ethyl acetate (2×100 mL). The combined organic extracts were washed with brine (50 mL), dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo. Trituration of the solid with 4% ethyl acetate/methylene chloride (25 mL) afforded the title compound as a yellow solid (1.091 g, 87%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07910595B2 |
| Quelldatensatz | uspto-grants-2011_03 |
| ORD ID | ord-f6cd7585c1f84199a0a4c25985e5e4a4 |
| Quellennotiz | uspto-grants-2011_03 |