HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → 4-(4-Chlorophenoxy)pyridin-3-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 4-(4-Chlorophenoxy)-3-nitropyridine | HCID 52840192 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | 4-(4-Chlorophenoxy)pyridin-3-amine | HCID 28890154 | 75% |
Reaction Steps
To a refluxing mixture of iron powder (1.91 g, 34.43 mmol) and ammonium chloride (230 mg, 4.30 mmol) in ethanol (45 μL) and water (8 mL) was added 4-(4-chlorophenoxy)-3-nitropyridine (AMR01116, 1.57 g, 6.26 mmol) and the resulting mixture was stirred at reflux for 1 h. After removal of the solvent, the residue was diluted in aqueous sodium hydrogen carbonate (40 mL) and extracted with DCM (3×20 mL). The organic layer was dried (MgSO4), filtered and evaporated. Flashmaster chromatography of the crude product using DCM/MeOH 9:1 as eluent gave 4-(4-chlorophenoxy)-pyridin-3-ylamin (1.03 g, 75%) as a white solid, mp 104-106° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08119627B2 |
| Source dataset | uspto-grants-2012_02 |
| ORD ID | ord-c69ddf6a6ac64b37a27d8da846da1077 |
| Source note | uspto-grants-2012_02 |