HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid → Ethyl 2-(3-bromo-2-chloro-4,5-difluorobenzoyl)acetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | Diethyl 2-(3-bromo-2-chloro-4,5-difluorobenzoyl)malonate | HCID 14071798 | — |
| Solvent | Water | HCID 962 | — |
| Product | Ethyl 2-(3-bromo-2-chloro-4,5-difluorobenzoyl)acetate | HCID 14071799 | 48.3% |
Reaction Steps
To an emulsion of diethyl 2-(3-bromo-2-chloro-4,5-difluorobenzoyl)malonate (11.44 g) in water (16 ml) was added p-toluenesulfonic acid (15 mg) and refluxed for 3 hours with stirring vigorously. After cooling, the reaction mixture was extracted with dichloromethane. The organic layer was washed with water, dried over anhydrous sodium sulfate and concentrated. The residue was purified by silica gel chromatography eluting with dichloromethane-n-hexane (1:1) to give the title compound (4.56 g), mp 47°-51° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04788320 |
| Source dataset | uspto-grants-1988_11 |
| ORD ID | ord-6e7b985b56334e989f4dd9c101437b89 |
| Source note | uspto-grants-1988_11 |