HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid → Ethyl 3-bromo-2,4,5-trifluorobenzoylacetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | Diethyl 3-bromo-2,4,5-trifluorobenzoylmalonate | HCID 13748803 | — |
| Solvent | Water | HCID 962 | — |
| Product | Ethyl 3-bromo-2,4,5-trifluorobenzoylacetate | HCID 10592111 | 56.8% |
Reaction Steps
To an emulsion of diethyl 3-bromo-2,4,5-trifluorobenzoylmalonate (3.25 g) in water (4 ml) was added p-toluenesulfonic acid (4 mg) and refluxed for 3 hours with vigorous stirring. After cooling, the reaction mixture was extracted with dichloromethane (8 ml×4). The organic layer was washed with water saturated with sodium chloride, dried over anhydrous sodium sulfate and concentrated. The residue was recrystallized from dichloromethane-n-hexane to give the title compound (1.51 g), mp 85°-88° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04826982 |
| Source dataset | uspto-grants-1989_05 |
| ORD ID | ord-11dcdb26c38a4600b3271fdecf8009a9 |
| Source note | uspto-grants-1989_05 |