HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylamine → HCID 21196241, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylamine | HCID 674 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | 5-Bromo-2-fluorobenzoic acid | HCID 2736315 | — |
| Catalyst | Dimethylformamide | HCID 6228 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 21196241 | HCID 21196241 | — |
Reaction Steps
A suspension of 2-fluoro-5-bromobenzoic acid (680 mg, 3.10 mmol) in methylene chloride (20 ml) was treated with oxalyl chloride (0.35 ml, 4.04 mmol), followed by four drops of N,N-dimethylformamide. The resulting clear solution was stirred for about three hours. The solvents were removed in vacuo and the residue was redissolved in methylene chloride and treated with dimethylamine (4.6 ml, 9.3 mmol). Stirring was continued for 18 hours. The reaction mixture was diluted with methylene chloride, and washed with saturated sodium bicarbonate and brine. The organic fraciton was dried over sodium sulfate, and the solvents were removed in vacuo. The desired title product was further purified by liquid chromatography.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06245761B1 |
| Source dataset | uspto-grants-2001_06 |
| ORD ID | ord-0dd86a7711074aeeab49e7d270a5b378 |
| Source note | uspto-grants-2001_06 |