HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → Methyl 2-fluoro-6-iodobenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | 2-Fluoro-6-iodobenzoic acid | HCID 2733302 | — |
| Catalyst | Dimethylformamide | HCID 6228 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Methyl 2-fluoro-6-iodobenzoate | HCID 12192164 | — |
Reaction Steps
Oxalyl chloride (2.5 ml, 28.66 mmol, 1.5 eq.) was added at room temperature to a suspension of 2-fluoro-6-iodobenzoic acid (5.1 g, 19.17 mmol, 1 eq.) in 40 ml of dry DCM under nitrogen atmosphere. A few drops of dry DMF were added and the mixture was stirred at room temperature for 1 h. The solvent was removed by distillation. The obtained residue was taken up in acetonitrile, which was distilled again, to remove excess acidity. The resulting brown oil was dissolved in dry DCM and the resulting solution was dropwise added to a suspension of potassium carbonate (7 g, 50.6 mmol, 2.6 eq.) in 20 ml of dry methanol. The reaction mixture was then stirred at room temperature overnight.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09062033B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-1f13627598b041dba4ae8b9661d3fb66 |
| Source note | uspto-grants-2015_06 |