HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethyl Acetate → 3,5,6-trifluoro-N1-(2-fluoro-4-iodophenyl)benzene-1,2-diamine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethyl Acetate | HCID 8857 | — |
| Edukt | Ammonium Chloride | HCID 25517 | — |
| Edukt | 2,3,5-trifluoro-N-(2-fluoro-4-iodophenyl)-6-nitroaniline | HCID 57430072 | — |
| Katalysator | Iron | HCID 23925 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | 3,5,6-trifluoro-N1-(2-fluoro-4-iodophenyl)benzene-1,2-diamine | HCID 59386343 | 66,4% |
Reaktionsschritte
To the stirred solution of (2-fluoro-4-iodo-phenyl)-(2,3,5-trifluoro-6-nitro-phenyl)-amine 3 (5.2 gm, 12.62 mmol) in EtOH (200 ml), ammonium chloride (10.12 gm, 189.3 mmol) and iron powder (10.57 gm, 189.3 mmol) was added. This reaction mixture was kept stirring at reflux for 16 hours. Reaction mixture was allowed to cool and was filtered over celite and concentrated to dryness. The residue obtained was taken into EtOAc and was washed with water. The EtOAc layer was dried over sodium sulfate and further purified by crystallization from EtOH to provide off-white solid (3.2 gm, yield: 66.39%). M−H+: 381.1. 1H NMR (DMSO, 300 MHz): 5.0 (s, 2H); 6.2 (t, 1H); 7.2-7.3 (m, 2H); 7.45 (s, 1H); 7.5 (d, 1H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08101799B2 |
| Quelldatensatz | uspto-grants-2012_01 |
| ORD ID | ord-4900108a9d1942c9bd23f96d841ca238 |
| Quellennotiz | uspto-grants-2012_01 |