HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 2-(p-Methoxybenzyl)-1,3,3-trimethyl-4-piperidone hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methyl 2-(p-methoxybenzyl)-4-oxo-1,3,3-trimethyl-5-piperidinecarboxylate | HCID 21448635 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | 2-(p-Methoxybenzyl)-1,3,3-trimethyl-4-piperidone hydrochloride | HCID 20474682 | 87% |
Reaction Steps
A solution of the hydrochloride (80 g) of methyl 2-(p-methoxybenzyl)-4-oxo-1,3,3-trimethyl-5-piperidinecarboxylate in 450 ml of 1 N hydrochloric acid is refluxed for 12 hours. After cooling, some resinous material is removed by extraction with ether. Alkalinization of the aqueus solution with the aid of ammonia causes the separation of the piperidone which is extracted with ether. Concentration in vacuo of the extent gives a residue which is dissolved in ethanolic hydrogen chloride. Evaporation of the ethanol leaves a syrupy residue which is dissolved in acetone, whereafter the crystalline hydrochloride separates. Yield 87%. Melting point 168° - 170° C, with decomposition.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04012392 |
| Source dataset | uspto-grants-1977_03 |
| ORD ID | ord-9aabc34d04624859928ec041e070f79f |
| Source note | uspto-grants-1977_03 |