HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → 5,6-difluoro-N1-(2-fluoro-4-iodophenyl)-3-methoxybenzene-1,2-diamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 2,3-Difluoro-N-(2-fluoro-4-iodophenyl)-5-methoxy-6-nitroaniline | HCID 59386312 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 5,6-difluoro-N1-(2-fluoro-4-iodophenyl)-3-methoxybenzene-1,2-diamine | HCID 53260966 | 90.3% |
Reaction Steps
To a stirred solution of (2,3-difluoro-5-methoxy-6-nitro-phenyl)-(2-fluoro-4-iodo-phenyl)-amine (0.57 gm, 1.34 mmol) ethanol (20 ml), ammonium chloride (1.18 gm, 20.16 mmol) and iron powder (1.15 gm, 21.44 mmol) were added. This reaction mixture was kept stirring at reflux for 16 hours. The reaction mixture was allowed to cool and was filtered over celite and concentrated to dryness. The residue obtained was taken into ethyl acetate and was washed with water. The organic layer was dried over sodium sulfate and further purified by crystallization from ethanol to provide an off-white solid (0.47 gm, yield: 90.3%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07842836B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-8ac55b51d5b2495a8be88dab3d51c7d8 |
| Source note | uspto-grants-2010_11 |