HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 86663960, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 86663961 | HCID 86663961 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 86663960 | HCID 86663960 | 97% |
Reaction Steps
To a solution of 2-(5-bromo-4-fluoro-2-iodo-3-nitrophenyl)pyridine (1.0 g, 2.36 mmol) in MeOH (25 mL) was added Fe powder (0.66 mL, 11.82 mmol) at 0° C. The mixture was stirred at rt for 10 min followed by addition of aqueous solution of NH4Cl (0.63 g, 11.82 mmol). The mixture was then heated up to 80° C. for 2 h. After completion of reaction (by TLC), the mixture was poured onto 100 mL of ice cold water and extracted with EtOAc (3×100 mL). The combined organic layer was washed with brine, dried over anhydrous Na2SO4 and solvent evaporated under reduced pressure. The crude residue was purified over 100-200 M silica-gel by using 6% EtOAc:hexane to obtain the desired product as a white solid (0.90 g, 97%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09181234B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-bb2c82ada2334a169b06378f9bc459c7 |
| Source note | uspto-grants-2015_11 |