Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Benzonitrile | HCID 7505 | — |
| Reactant | Potassium ethylmalonate | HCID 86617294 | — |
| Catalyst | Zincchloride | HCID 3007855 | — |
| Product | Ethyl benzoylacetate | HCID 7170 | 75% |
Reaction Steps
To 100 □ of 1,2-dichloroethane were added 5.5 □ of benzonitrile, 7.2 g of zinc chloride, and 11 g of potassium ethylmalonate, and then the mixture was stirred at reflux. After the reaction was completed, 100 □ of 6 N hydrochloric acid was added to the mixture, which then was stirred at reflux at 90° C. for 1 hour. After confirming completion of the reaction by TLC, the solution was cooled to 20° C., and then an organic layer was separated therefrom. The organic layer was concentrated through distillation under reduced pressure. Thus resulted residue was purified by silica gel column chromatography (eluent: ethylacetate/n-hexane=1/20, v/v) to obtain the title compound in the yield of 75% (7.6 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07642356B2 |
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| Source dataset | uspto-grants-2010_01 |
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| ORD ID | ord-45934e01d91a49cb9462ce9b1839f454 |
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| Source note | uspto-grants-2010_01 |
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