HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → N-(5-bromo-2-pyridinyl)-(2-nitro)-5fluorophenylcarboxamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 2-Amino-5-bromopyridine | HCID 70622 | — |
| Reactant | 5-Fluoro-2-nitrobenzoic acid | HCID 2737420 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | N-(5-bromo-2-pyridinyl)-(2-nitro)-5fluorophenylcarboxamide | HCID 22596298 | 68.1% |
Reaction Steps
A solution of 5-fluoro-2-nitrobenzoic acid (10.0 g, 54 mmol, 1.0 equiv), 2-amino-5-bromopyridine (12.2 g, 1.3 equiv), in 80 mL of pyridine was treated with phosphorous oxychloride (25.3 g, 3.0 equiv) for 30 min. The volatile was evaporated and the residue was redissolved into EtOAc, washed with 1N HCl, saturated aqueous NaHCO3 and saturated aqueous NaCl. The organic layer was dried over Na2SO4, filtered, and evaporated. The volatile was evaporated, and the product was triturated with diethyl ether to give N-(5-bromo-2-pyridinyl)-(2-nitro)-5-fluorophenylcarboxamide (12.5 g, 68%). MS found for C12H7BrFN3O3 (M+H)+: 340, 342.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07727982B2 |
| Source dataset | uspto-grants-2010_06 |
| ORD ID | ord-b7fdc228ba5a4a11b5ad77c59bddf049 |
| Source note | uspto-grants-2010_06 |