HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 68717432, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Piperidine | HCID 8082 | — |
| Reactant | Ethyl Acetoacetate | HCID 8868 | — |
| Reactant | 4-Formyl-3-methoxybenzonitrile | HCID 16659251 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68717432 | HCID 68717432 | — |
Reaction Steps
3 g (18.61 mmol) of 4-formyl-3-methoxybenzonitrile, 2.6 ml (20.47 mmol) of ethyl 3-oxobutanoate, 1.33 ml (23.26 mmol) of acetic acid and 0.18 ml (1.85 mmol) of piperidine are stirred in 70 ml of dry dichloromethane under reflux with a water trap for 24 h. After cooling, the reaction solution is washed successively with saturated sodium bicarbonate solution and saturated sodium chloride solution. The organic phase is dried over magnesium sulfate and concentrated. The residue is recrystallized from diethyl ether. 5.01 g (98% of theory) of the title compound are obtained as E/Z isomer mixture in the form of a pale yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08399471B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-5e3179b77d3c4d4e84178d5b416928b5 |
| Source note | uspto-grants-2013_03 |