HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 297403, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | 2-Chlorobenzaldehyde | HCID 6996 | — |
| Reactant | Ethyl Acetoacetate | HCID 8868 | — |
| Catalyst | Piperidine | HCID 8082 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 297403 | HCID 297403 | 98.1% |
Reaction Steps
A mixture of 25.0 g of 2-chlorobenzaldehyde, 23.1 g of ethyl acetoacetate, 2.1 g of acetic acid and 0.6 g of piperidine in 100 cc of benzene was heated under reflux for 8 hours and removed water by a Dean-Stark trap. After cooling, to the reaction mixture was added ethylacetate and water. The organic layer was further washed with a saturated aqueous sodium chloride solution and dried over magnesium sulfate. The solvent was distilled off and the crude product thus obtained was purified by a silica gel column chromatography (eluent: ethyl acetate/hexane=1/9) to obtain 44.0 g of compound A. Yield: 97.9%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05500424 |
| Source dataset | uspto-grants-1996_03 |
| ORD ID | ord-68f4ca5e872949d6bcac812ee1701a1a |
| Source note | uspto-grants-1996_03 |