HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → methyl N-(p-methoxybenzyl)nipecotate hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Methyl piperidine-3-carboxylate | HCID 351626 | — |
| Reactant | (4-Methoxyphenyl)methyl trichloroacetate | HCID 13548121 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | methyl N-(p-methoxybenzyl)nipecotate hydrochloride | HCID 14181476 | 63.8% |
Reaction Steps
A mixture of 23 g of methyl nipecotate, 24.3 g of potassium carbonate, and 52 g of p-methoxybenzyl trichloroacetate in 800 ml of toluene is refluxed under nitrogen for seventy-two hours. The mixture is cooled, the toluene removed in vacuo, the residue dissolved in chloroform, and this solution washed once with 400 ml of aqueous potassium carbonate and then with 400 ml of 10% hydrochloric acid. The chloroform solution is dried and concentrated in vacuo to a viscous brown oil. Trituration of this oil with ethyl acetate affords 30.7 g of methyl N-(p-methoxybenzyl)nipecotate hydrochloride as an off-white crystalline solid. Recrystallization from ethyl acetate yields the analytical sample, m.p. 150°-154°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04146611 |
| Source dataset | uspto-grants-1979_03 |
| ORD ID | ord-ffff98dc2c9540b4941eb19f1f073a0e |
| Source note | uspto-grants-1979_03 |