HuagongsheHuagongshe Chemistry Print Report · For research reference only
Piperidine → HCID 69590310, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Piperidine | HCID 8082 | — |
| Reactant | 3-Chlorobenzaldehyde | HCID 11477 | — |
| Reactant | 3-Phenyl-2-propen-1-yl 3-oxobutanoate | HCID 93726 | — |
| Reactant | Ammonium Acetate | HCID 517165 | — |
| Reactant | 2-Cyanoethyl prop-2-ynoate | HCID 20493224 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Benzene | HCID 241 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 69590310 | HCID 69590310 | — |
Reaction Steps
655 mg (3.0 mmol) of cinnamyl acetoacetate, 0.34 ml (3.0 mmol) of 3-chlorobenzaldehyde and 0.0297 ml of piperidine were heated under reflux in 3.0 ml of benzene overnight while water was removed. The reaction liquid was washed with water and then dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The obtained residue was heated to 70° C. together with 370 mg (3.0 mmol) of (2-cyanoethyl) propiolate and 232 mg (3.0 mmol) of ammonium acetate under stirring in 3 ml of acetic acid for two nights. Acetic acid was evaporated under reduced pressure, and the residue was purified by the silica gel chromatography (hexane/ethyl acetate=3/2) to obtain the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06995179B2 |
| Source dataset | uspto-grants-2006_02 |
| ORD ID | ord-0e300d8d7d0b4acfb11904bdc3326333 |
| Source note | uspto-grants-2006_02 |