HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → Methyl 5-chloro-2-fluorobenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | 5-Chloro-2-fluorobenzoic acid | HCID 2736537 | — |
| Catalyst | Dimethylformamide | HCID 6228 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Methyl 5-chloro-2-fluorobenzoate | HCID 21525433 | 92% |
Reaction Steps
To a suspension of 5-chloro-2-fluoro-benzoic acid (2.0 g, 11.5 mmol) in dichloromethane (50 ml) was added a solution of oxalyl chloride in dichloromethane (2 M, 6.5 ml, 13 mmol) followed by N,N-dimethylformamide (5 drops). After stirring for 1 hour, methanol (10 ml) was added. After stirring for 20 hours, the mixture was concentrated under reduced pressure. The residue was partitioned between ethyl acetate (200 ml) and saturated aqueous potassium carbonate solution (100 ml). The organic layer was dried over sodium sulfate and concentrated under reduced pressure to provide methyl 5-chloro-2-fluoro-benzoate (2.0 g, 92% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07291616B2 |
| Source dataset | uspto-grants-2007_11 |
| ORD ID | ord-b751df6b38f941d4be9eb063461acba0 |
| Source note | uspto-grants-2007_11 |