HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → Methyl 2-chloro-4,5-difluorobenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | 2-Chloro-4,5-difluorobenzoic acid | HCID 737171 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | Methyl 2-chloro-4,5-difluorobenzoate | HCID 22149760 | 84% |
Reaction Steps
To a stirred suspension of 5.0 g (26 mmol) 2-Chloro-4,5-difluoro-benzoic acid (Apollo) and 50 ml methanol were added 7.41 ml (104 mmol) acetyl chloride drop wisely at 0° C. The reaction mixture was stirred over night, filtered and concentrated. The residue was diluted with dichloromethane, washed with diluted sodium hydrogen carbonate solution, dried with sodium sulphate and concentrated. The residue was purified by column chromatography (hexane:ethylacetate). The desired product 22a was obtained in 84% yield (4.51 g, 21.8 mmol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08557776B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-d8190e6abcb7421199a5d4e7f0654226 |
| Source note | uspto-grants-2013_10 |