Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetone | HCID 180 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Diethyl bromomalonate | HCID 69637 | — |
| Reactant | HCID 15214193 | HCID 15214193 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 10266436 | HCID 10266436 | — |
Reaction Steps
A mixture of 2-benzoyl-4,5-dimethylbenzoic acid (11.4 g), acetone (300 ml), dimethylformamide (10 ml), potassium carbonate (6.83 g) and diethyl bromomalonate (12.84 g) was stirred at room temperature for 60 hours. The solvent was then distilled off and ethyl acetate was added to the residue. The mixture was washed with water and dried (Na2SO4) and the solvent was distilled off. To the residue were added acetic acid (180 ml) and hydrochloric acid (180 ml) and the mixture was heated at 110° C. for 5 hours. The reaction mixture was then concentrated and the concentrate was diluted with water and extracted with ethyl acetate. The extract was washed with water and dried (Na2SO4) and the solvent was distilled off. The resulting crystals were recrystallized from ethyl acetate-isopropyl ether to provide the title compound. Melting point: 265°-268° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05523305 |
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| Source dataset | uspto-grants-1996_06 |
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| ORD ID | ord-a2bcc79351f14c3d95d29cacb992c3f7 |
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| Source note | uspto-grants-1996_06 |
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