Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium amide | HCID 24532 | — |
| Reactant | 2-Fluoro-4-iodoaniline | HCID 185694 | — |
| Reactant | 2,4,5-Trifluorobenzoic acid | HCID 521170 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 22286045 | HCID 22286045 | 43.5% |
Reaction Steps
2,4,5-Trifluorobenzoic acid (643 mg, 3.65 mmol) and 2-fluoro-4-iodoaniline (1.0 g, 4.22 mmol) were taken into acetonitrile (30 mL) followed by addition of lithium amide (290 mg, 12.7 mmol) and the mixture was heated to 60° C. under a nitrogen atmosphere for one hour. On cooling to room temperature the mixture was added to 1 N aqueous hydrochloric acid (100 mL) and the precipitate formed was collected by filtration and washed once with water then hexanes and dried in vacuo to give 4,5-difluoro-2-[(2-fluoro-4-iodophenyl)amino]benzoic acid (624 mg, 43% yield) as a tan solid. 1H-NMR (400 MHz, D6-DMSO): 13.65 (br s, 1H), 9.63 (s, 1H), 7.84 (tr, 1H), 7.71 (d, 1H), 7.52 (d, 1H), 7.32 (tr, 1H), 7.03-6.98 (dd, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07999006B2 |
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| Source dataset | uspto-grants-2011_08 |
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| ORD ID | ord-5ba27e1e946d4c349fa5196f83a978e8 |
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| Source note | uspto-grants-2011_08 |
|---|